Practical 

Flavoring  Extract 
Maker 


By 

E.  J.  JCESSLER 

A  TREATISE  ON  THE  MANU- 
FACTURE OF  THE  PRIN- 
CIPAL FLAVORING  EX- 
TRACTS, IN  ACCORDANCE 
WITH  THE  REQUIREMENTS 
OF  THE  FOOD  LAWS  OF 
THE  UNITED  STATES ; 
WRITTEN  BY  A  PRACTI- 
CAL MANUFACTURER  WHO 
SETS  DOWN  THE  FULL 
KNOWLEDGE  OF  HIS5  SFE-' 
CIALTY  ACQUIRED  DURING 
MANY  YEARS  OF  CONTIN- 
UOUS EXPERIENCES''"' 


1912 
The  Spice  Mill  Publishing  Co. 

NEW  YORK 


COPYRIGHT,    1912  BY 
THE  SPICE  MILL  PUBLISHING  Co. 

NEW  YORK 


Main  Lib. 

AGRIC, 


DtPt.  ^^ 


Table  of  Contents 


GENERAL  OBSERVATIONS        ....  6 

QUALIFICATIONS  OF  A  MANUFACTURER    .         .  7 

WHAT  CONSTITUTES  A  FLAVORING  EXTRACT    .  8 

MANUFACTURE  OF  VANILLA  EXTRACTS 

Description  of  Varieties  of  Vanilla  Beans — 
Resins — Selecting  Beans — Bean  Storage — Cut- 
ting Beans — Exhaustion  of  the  Vanilla  Bean — 
Tonka  Extract — Imitation  Vanilla  Extracts — 
Non-Alcoholic  Extracts — Testing  Vanilla 
Extracts  ......  10-31 

MANUFACTURE  OF  LEMON  EXTRACTS 

Terpeneless      Extract      of      Lemon — Lemon 

Flavor,  Imitation — Extract  of  Orange  .          32-41 

VARIOUS  EXTRACTS 

Extracts  of  Almond,  Wintergreen,  Pepper- 
mint, Ginger,  Rose,  Allspice  (Pimento), 
Anise,  Celery,  Cinnamon,  Cassia,  Cloves, 
Mint  (Spearmint),  Chocolate,  Sarsaparilla 
(imitation),  Pistachio  (imitation) — Ethereal 
imitation  Flavors  .....  42-51 

LABORATORY  NOTES 

Menstruums  (solvents) — Rules  for  Testing 
Alcohol,  Oils,  etc. — Filtration — Double  Pres- 
sure Filter  and  Percolator — Testing  Methods — 
Estimation  of  Small  Quantities  of  Essential 
Oils — To  Determine  per  cent,  of  gas  in  Aqua- 
Ammonia,  and  per  cent,  of  Acidity  of  Vinegar 
—To  Purify  Essential  Oils  .  .  .  52-66 

MISCELLANEOUS  RECEIPTS     ....  67-69 

ADHESIVES 70 

WEIGHTS  AND  MEASURES,  TABLES  ...  71 

HOUSEHOLD  AMMONIA          ....  72 

BOTTLES  AND  CORKS     .         .         .         .         .  73-76 

FIGURING  COSTS 76-79 

INDEX 80-83 

443166 


General  Observations 

PRIOR  to  the  enactment  of  the  State  and  Federal 
pure   food  laws,   few   classes   of   food  products 
were    so    grossly    adulterated    as    flavoring    ex- 
tracts.     Some   of   the   compounds   termed    "ex- 
tract of  vanilla"  were  manufactured  at  a  cost 
of   from  40  to  60  cents  per  gallon.     This  con- 
dition undoubtedly  resulted  from  the  ease  with  which 
substitutes  that  readily  deceive  the  purchaser  are  pre- 
pared.    The  average  manufacturer  was  by  no  means  in- 
spired by  the  desire  to  adulterate ;  in  the  majority  of  in- 
stances the  causes  of  the  decline  in  the  quality  of  the 
extracts  offered  can  be  traced  directly  to  the  door  of 
either  the  dealer  or  consumer,  or  both.     In  justice  to  the 
manufacturer,  it  may  be  stated  that  the  rule  of  price 
regulating  quality  was  generally  observed.    This  rule,  al- 
though holding  good   in  the  main,  has  its   exceptions. 
The  discussion,  while  not  having  a  direct  bearing  on  the 
manufacture  of  flavoring  extracts,  is  of  sufficient  impor- 
tance, especially  when  the  manufacturer  is  called  upon  to 
match  goods  offered  by  competitors;  and  in  order  to 
properly  decide  such  problems,  he  should  have  a  fair 
knowledge  of  the  non-technical  processes  for  conducting 
tests. 


QUALIFICATIONS  OF  A  MANUFACTURER. 

The  primary  qualifications  of  an  extract  manufac- 
turer are  embraced  in  an  ordinary  education,  plus  a 
liberal  display  of  effort.  One  need  not  be  a  graduate 
chemist,  although  a  knowledge  of  the  fundamental  prin- 
ciples of  chemistry  will  prove  a  valuable  aid.  For  the  be- 
ginner, in  the  absence  of  a  better  opportunity,  the  writer 
will  suggest  that  he  study  a  chemical  text  book  such  as 
"Steele's  Popular  Chemistry."  Too  much  importance 
cannot  be  attached  to  the  necessity  of  familiarizing  one's 
self  with  both  the  Federal  and  State  food  laws,  and  the 
author  would  suggest  that  one  request  from  the  Secre- 
tary of  the  United  States  Department  of  Agriculture  the 
mailing  to  him  of  all  printed  matter  having  reference  to 
the  Federal  Food  Law  requirements,  including  circular 
No.  19,  "Standards  of  Purity  for  Food  Products,"  and 
also  to  place  his  firm  name  on  the  mailing  list  for  "No- 
tices of  Judgment,"  the  latest  rulings,  etc.,  and  adhere 
to  the  Department's  teachings  religiously.  The  same 
course  should  be  followed  in  respect  to  the  State  or 
States  in  which  one's  products  are  offered  for  sale.  In 
the  event  of  his  inability  to  interpret  the  laws,  it  will  be 
best  to  employ  the  services  of  a  competent  attorney. 

One  should  never  entertain  the  idea  that  his  particu- 
lar process  or  system  is  perfect  and  he  should  not  forget 
that  perfection  is  an  impossibility  and  that  true  progress 
is  from  the  less  to  the  greater.  It  requires  energy  and 
push  to  make  headway  in  the  world,  and  since  work  is 
ordinarily  the  measure  of  success,  an  active,  energetic 
and  persevering  man  is  sure  to  succeed. 


8  What  Constitutes  a  Flavoring  Extract 

WHAT  CONSTITUTES  A  FLAVORING 
EXTRACT? 

The  best  definition  is  contained  in  Circular  No.  19,  of 
the  United  States  Department  of  Agriculture,  as  follows : 

"A  flavoring  extract  is  a  solution  in  ethly  alcohol  of 
proper  strength  of  the  sapid  and  odorous  principles  de- 
rived from  an  aromatic  plant,  or  parts  of  the  plant,  with 
or  without  its  coloring  matter,  and  conforms  in  name  to 
the  plant  used  in  its  preparation." 

This  definition  excludes  all  preparations  which  are 
not  solutions  in  alcohol  and  eliminates  the  various  forms 
of  flavored  sugars  which  are  quite  extensively  used 
abroad. 

Extracts  are  divided  into  four  classes,  as  follows : 

1.  Those  obtained  by  maceration  and  percolation  of 
beans,  seeds,  roots,  leaves  and  fruit  of  the  plants. 

2.  Those  obtained  by  soltuion  of  essential  oils. 

3.  Those  obtained  by  solution  of  synthetics   (imita- 
tions), such  as  vanillin,  and  coumerin  tinctures. 

4.  Those  obtained  by  solution  of   compound  esters 
(a  compound  ether  derived  from  an  oxygenated  acid). 

First  Class.  The  following  extracts  are  included  un- 
der the  first  class :  Vanilla,  Tonka,  Ginger,  Celery,  etc. 

Second  Class.  Lemon  extract ;  Terpeneless  lemon  ex- 
tract; Orange  extract;  Terpeneless  orange  extract;  Cin- 
namon extract ;  Cassia  extract ;  Almond  extract ;  Pepper- 
mint extract;  Wintergreen  extract;  Nutmeg  extract; 
Rose  extract ;  Anise  extract ;  Celery  extract ;  and  Thyme 
extract. 

Third  Class.  Under  the  third  class  are  included  ex- 
tracts as  follows :  Vanillin  extract,  the  synthetic  prin- 
ciple of  the  vanilla  bean ;  coumarin  extract,  the  synthetic 
principle  of  the  tonka  bean ;  imitation  wintergreen  ex- 


What  Constitutes  a  Flavoring  E^tiact  _  o 

tract,  methyl  salicylate,  the  synthetic  principle  of  oil  of 
wintergreen;  imitation  almond,  benzaldehyde,  the  syn- 
thetic principle  of  oil  of  bitter  almonds ;  imitation  sassa- 
fras, safrol,  the  synthetic  principle  of  oil  of  sassafras. 

Fourth  Class.  Under  this  class  are  included  extracts 
as  follows :  Imitation  pineapple,  strawberry,  banana, 
raspberry,  apple,  cherry  and  peach — all  ethereal  products 
representing  ethyl  butyrate,  amyl  butyrate,  ethyl  for- 
mate, amyl  acetate,  ethyl  acetate,  and  amyl  valerinate,  all 
blended  in  proportions  to  represent  the  various  flavors 
desired. 


io  '     .Manufacture  of  Vanilla  Extracts 


VANILLA  EXTRACTS 


VANILLA  BEANS. 

The  vanilla  bean,  being  the  source  of  the  most  im- 
portant and  popular  flavoring  on  the  market,  will  first 
be  considered.  The  bean-producing  plant  is  a  climbing 
parasite  (the  Vanilla  planifolia  of  Andrews).  It  was 
first  described  by  a  Franciscan  Friar  in  1575,  and  at  that 
time  was  supposed  to  be  of  great  medicinal  value.  The 
bean  is  a  native  of  Mexico,  the  West  Indies,  South  Amer- 
ica, the  Bourbon  Isles  (chiefly  the  Comores  group),  Re- 
union, Seychelle,  Madagascar,  and  the  East  Indies. 

Vanilla  beans  on  the  market  are  of  various  kinds  as 
to  name  and  quality.  We  have  the  Mexican,  Bourbon, 
imitation  Mexican,  Tahiti,  Guatemala,  Java,  and'Vanillon 
or  Wild  Vanilla.  In  quality  we  find  quoted:  ordinary; 
fair;  good;  extra;  split;  cuts;  broken  lots  of  mixed 
lengths ;  and  powdered  with  50  per  cent,  of  sugar.  Thus 
we  have  various  grades,  from  which  no  one  can  fail  to 
find  his  Jiking,  either  in  price  or  quality.  In  England 
manufacturers  use  the  Bourbon  Beans  almost  exclusively, 
using  the  Seychelle  variety,  Seychelle  being  an  English 
province.  France  naturally  is  very  partial  to  the  Bour- 
bons and  Mexicans,  while  Germany  is  very  partial  to  the 
Tahiti.  The  Germans  do  not  make  extract,  but  sell  va- 
nilla beans  by  the  piece,  these  pieces  being  boiled  with  the 
pudding,  etc. ;  the  consequence  is  that  the  Germans  want 
as  many  beans  as  possible  for  the  price  per  pound,  and 
they  naturally  purchase  the  Tahiti  grade. 

The  United  States,  among  the  nations,  is  by  far  the 


Description  of  Varieties  of  Vanilla  Beans  n 


largest  consumer  of  vanilla  beans,  the  two  most  popular 
grades  being  the  Mexicans  and  Bourbons,  although  of 
late  the  Tahiti  is  being  more  extensively  used  in  various 
blends. 


DESCRIPTION   OF  VARIETIES   OF   VANILLA 
BEANS. 

The  first  quality  of  Mexican  beans  occurs  in  pods  of 
from  8  to  10  inches  long,  flattened,  ^  to  ^  inches  in 
diameter,  with  the  lower  end  slightly  tapered,  the  upper 
end  gradually  tapering  for  about  a  quarter  the  length  of 
the  pod,  and  is  usually  curved  and  slightly  twisted  near 
the  point.  The  color  is  dark  brown,  the  pods  plump,  the 
surface  rigid  longitudinally  and  frequently  containing  an 
incrustation  of  fine  crystals  beginning  at  the  ends,  grad- 
ually extending ;  when  fresh,  somewhat  viscid,  but  always 
roughish  to  the  touch. 

The  Bourbon  vanilla  resembles  the  Mexican,  but  is 
scarcely  so  long  in  the  tapering  portions;  is  of  a  dark 
brown,  almost  black  color;  is  not  as  firm  as  the  Mexi- 
can ;  has  a  smooth  and  waxy  surface  and  frequently  be- 
comes covered  with  a  coating  of  needle-shaped  crystals 
(vanillin)  known  as  "frost." 

The  Seychelles  and  Mauritius  vanilla  has  the  pods 
6  inches  in  length,  not  over  %  inch  in  width,  and  is 
characterized  by  the  pale  color,  the  faint  odor  and  a 
smooth  but  not  waxy  surface. 

Guadeloupe  vanilla  is  usually  recognizable,  when  the 
bean  is  entire,  by  it  being  broad  arid  flattened,  usually 
y2  inch  or  more  wide,  slightly  tapering  at  the  lower  end 
and,  at  the  upper,  sharply  tapering  an  inch  or  so  at  the 
point.  It  has  a  reddish  brown  color  and  possesses  an 


12  Manufacture  of  Vanilla  Extracts 


inferior  pungent  odor.  It  is  very  pulpy,  with  a  surface 
intermediate  between  the  Bourbon  and  the  Mexican,  and 
has  but  few  crystals.  One  variety  of  this  vanilla,  sold 
under  the  name  of  "Vanillons,"  possesses  the  odor  of 
heliotrope  and  is  used  principally  by  perfumers  and  to- 
bacco manufacturers. 

Java  vanilla,  which  is  almost  exclusively  consumed 
in  Holland,  has  a  pod  from  4  to  6  inches  long,  and  has 
a  flavor  almost  as  fine  as  that  of  the  Mexican  bean  and 
a  much  stronger  odor. 

Tahiti  vanilla  (transplanted  Mexicans)  has  its  pods 
from  4  to  7  inches  long,  is  flat,  from  ^  to  l/2  inch 
wide,  and  has  a  slightly  reddish  brown  color.  Owing  to 
the  insufficient  attention  of  the  vanilla  planters  (mostly 
Chinese)  of  the  Society  Islands  (Tahiti  being  the  ship- 
ping port)  to  the  curing  of  the  beans  and  the  indiscrim- 
inate sale  of  their  entire  crop  without  regard  to  maturity, 
the  value  of  the  Tahitian  vanilla  has  been  depreciating 
in  the  world's  markets;  however,  since  the  vanilla  laws, 
which  went  into  effect  April  i,  1911,  providing  means 
for  licensing  the  curers  and  a  rigid  inspection  of  the 
beans  prior  to  shipment,  the  character  of  this  grade  of 
vanilla  has  been  very  materially  improved  and  is  being 
extensively  employed  in  this  country.  Nearly  all  of  the 
Tahiti  vanilla  is  received  at  the  port  of  San  Francisco, 
Cal. 

An  interesting  incident  in  the  growth  of  vanilla  beans 
is  the  artificial  pollenization  of  the  flower.  Originally 
the  cultivators  depended  solely  upon  insects  to  transmit 
the  pollen  from  blossom  to  blossom,  the  results  being 
anything  but  satisfactory,  since  some  of  the  vines  were 
made  to  bear  too  many  pods,  while  others  too  few,  re- 
sulting in  a  loss  in  both  quality  and  quantity  of  the  fruit 
produced. 


Description  of  Varieties  of  Vanilla  Beans  13 

To  overcome  this  difficulty  the  planter  pollenizes  by 
hand,  the  operation  being  a  simple  one  and  accomplished 
by  removing  the  pollen  from  the  male  flowers  by  means 
of  a  splinter  of  wood,  about  the  size  of  a  tooth  pick,  and 
placing  small  portions  of  the  pollen  in  the  female  flowers. 
Since  the  flowers  open  during  the  night  and  close  before 
midday,  the  work  is  performed  in  the  early  morning  and 
is  most  successful  if  performed  on  the  first  day  on  which 
the  flower  blossoms.  Flowers  not  successfully  pollinated 
soon  wither  and  fall.  With  this  method  the  number  of 
pods  which  each  vine  is  maturing  can  be  ascertained 
and  controlled,  according  to  its  age  and  physical  struc- 
ture. 

The  fruit,  as  first  picked,  has  no  aroma,  the  vanillin 
during  the  process  of  curing  being  developed  from  the 
glucoside  conferin  in  the  interior  of  the  fruit.  When 
vanilla  beans  are  left  to  ripen  too  long,  the  pods  will 
split  and  deteriorate,  and  the  beans  are  then  either  sold 
as  "splits"  or  are  mixed  with  other  inferior  goods  and 
sold  as  "cuts."  The  sale  of  cuts  permits  of  considerable 
sophistication,  in  that,  frequently,  such  beans  as  Tahiti 
are  found  among  the  mixture.  Beans  that  have  been 
picked  too  early  are  likewise  distinctly  inferior. 

If  vanilla  beans,  finely  divided,  be  distilled  with  water, 
a  turbid  liquid  passes,  which  becomes  clear  by  agitation 
with  sulphuric  ether,  which  ether  on  evaporation  yields 
crystals  of  vanillin. 

Vanilla  beans,  from  which  the  vanillin  has  been  re- 
moved by  means  of  a  solvent,  are  sometimes  offered  to 
the  trade.  The  fraud  is  to  be  detected  by  the  absence 
of  the  flavor  and  odor.  Such  beans,  also  beans  of  an 
inferior  quality,  are  sometimes  "improved"  in  appear- 
ance and  in  odor  by  the  use  of  benzoic  acid. 

For  the  detection  of  this  fraud,  the  operator  should 


14  Manufacture  of  Vanilla  Extracts 


avail  himself  of  the  fact  that  while  benzoic  acid  crystals 
are  flattened  and  rhomboidal  and  generally  lie  upon  the 
bean,  those  of  vanillin  are  usually  needle-shaped  and 
stand  out  almost  at  right  angles  from  the  surface  of  the 
fruit.  These  indications  are  not  always  infallible,  since 
the  crystalline  structure  is  influenced  considerably  by 
the  temperature,  humidity  of  the  surrounding  air,  etc. 
To  more  accurately  determine  the  character  of  the  flat 
crystals,  detach  them  with  the  aid  of  a  knife  point,  place 
in  a  test  tube,  heat  over  a  Bunsen  burner,  and,  if  com- 
posed of  benzoic  acid,  the  unmistakable  irritating  odor 
of  benzoic  acid  may  be  detected. 

The  absence  of  the  crystalline  coating  on  the  vanilla 
beans  is  not  necessarily  an  indication  of  inferiority,  since 
high  grade  vanilla  beans  very  frequently  manifest  an  op- 
posite condition.  The  most  important  fragrant  principle 
of  the  vanilla  bean  and  true  vanilla  extract  is  vanillin 
(Methyprotocatechuic  aldehyde),  a  crystalline  compound, 
the  beans  containing  from  i  to  about  2^4  per  cent.  The 
practical  value  of  a  vanilla  bean  is  not,  by  any  means,  to 
be  determined  by  the  per  cent,  of  vanillin  content,  since 
it  frequently  occurs  that  the  very  finest  beans  will  show 
the  smallest  vanillin  content.  Busse  found  the  following 
percentages  of  vanillan : 

Mexican  vanilla  beans 1.69  to  1.86 

Bourbon  vanilla  beans 1.91  to  2.48 

Tahiti  vanilla  beans 2.00 

German  African  vanilla  beans... 2.16 
Java  vanilla  beans 2.75 

RESINS. 

While  vanillin  is  a  most  important  constituent  of 
vanilla  beans,  there  are  other  substances,  such  as  resins, 


Resins — Selecting  Vanilla  Beans  15 


gums,  etc.,  soluble  in  dilute  alcohol,  that  contribute  to 
the  fragrance  and  value  of  the  extract.  It  is  from  these 
resins  and  gums  that  the  vanilla  extract  derives  the 
greater  portion  of  the  dark  brown  color.  Practically 
nothing  at  this  time  is  known  of  the  chemical  constitu- 
ents of  vanilla  resins.  Experience  has  amply  proven  that 
to  extract  these  resins  thoroughly,  a  menstruum  of  at 
least  50  per  cent,  by  volume  of  alcohol  is  necessary. 

Vanilla  resins  are  a  valuable  analytical  index,  demon- 
strating approximately  if  the  correct  portion  of  beans  to 
menstruum  has  been  employed,  likewise  if  the  latter  was 
of  sufficient  strength  and  if  the  extracting  process  was 
thorough. 

According  to  Brooks,  the  amount  of  resin  present  in 
different  beans  is  as  follows  : 

Per  Cent. 

Mexican  (whole)   1.47 

Mexican  (cuts)  1.96 

Seychelle  (Bourbon  cured) 1.93 

Comoros    (Nossi  Bey) 1.96 

Comoros  (short) 1.90 

Mexican  and  South  American,  equal  parts .   2.56 

SELECTING  BEANS. 

In  purchasing  vanilla  beans  it  is  almost  a  necessity 
to  take  them  on  trust  as  to  quality.  The  question  of 
length  as  an  element  of  value  appears  now  to  be  ignored 
by  some  of  the  larger  buyers,  on  the  principle  that  the 
mere  length  of  the  bean  has  no  more  to  do  with  its  flavor 
or  flavoring  qualities  than  the  length  or  breadth  of  a 
man  decides  his  mental  or  moral  qualities ;  but  as  station, 
culture  and  education  all  play  their  part  in  the  forma- 
tion of  character,  so  soil,  climate  and  cultivation  estab- 


16  Manufacture  of  Vanilla  Extracts 


lish  the  quality  of  the  fruit  under  consideration.  To  be 
candid,  and  speaking  as  a  manufacturer,  we  need  more 
knowledge  on  the  relative  value  of  this  valuable  fruit, 
since  all  that  the  average  buyers  are  sure  of  in  pur- 
chasing are  the  price,  aroma  and  physical  structure ; 
therefore,  in  buying  vanilla  beans  one  should  try  to  deal 
with  the  most  reliable  concern  of  whom  he  has  knowl- 
edge. 

The  most  practical  method  to  pursue  in  purchasing 
beans  would  be  as  follows :  When  in  the  market  for 
beans,  request  from  your  dealer  or  dealers  quotations 
with  samples,  and  on  receipt  of  samples  proceed  to  make 
up  test  batches  with  the  aid  of  small  test  percolators,  or 
by  maceration  with  frequent  agitation,  being  careful  to 
employ  the  same  relative  quantity  of  beans  and  mens- 
truum strength  and  treatment  in  all  tests  under  operation. 
A  test  of  this  character  can  be  successfully  conducted 
within  a  period  of  forty-eight  hours.  When  completed, 
first  carefully  note  the  density  of  color ;  next  dealco- 
holize  in  a  porcelain  evaporating  dish  over  a  water  bath ; 
remove,  and  when  almost  cool,  determine  character  of 
aroma  by  the  sense  of  smell,  and  when  thoroughly  cool, 
by  the  sense  of  taste.  In  this  manner  you  will  be  in  a 
position  to  determine  the  .relative  values  of  the  samples 
submitted. 

BEAN  STORAGE. 

Beans  that  are  not  required  for  immediate  use  should 
be  stored  in  a  cool,  dry  store  room  and  should  be  ex- 
amined from  time  to  time  to  guard  against  the  forma- 
tion of  mold  or  other  infection.  Beans  can  be  success- 
fully stored  in  their  reduced  (cut)  state,  provided  they 
are  incorporated  with  sufficient  dilute  alcohol  (equal 
parts)  or  glycerin  +o  cover  them,  and  kept  in  an  air- 


Exhaustion  of  the  Vanilla  Bean  17 


tight  container  in  a  cool  place ;  but  do  not  forget  to  note 
on  the  package  the  exact  weight  of  the  beans,  also  the 
amount  of  dilute  alcohol  or  glycerin  used,  as  then  you 
will  be  enabled  to  determine  your  formula  more  correctly. 

CUTTING  BEANS. 

Vanilla  beans  should  always  be  cut,  not  ground,  for 
the  following  reasons :  Grinding,  in  every  instance,  is 
accompanied  with  a  rise  of  temperature,  and  it  is  a 
proven  fact  that  the  heating  of  vanilla  beans  results  in 
the  decomposition  of  the  greater  portion  of  the  highly 
flavored  aldehydes.  The  several  forms  of  "meat  cutters" 
that  are  sometimes  used  rip  and  shred  the  beans,  and, 
through  friction,  generate  considerable  heat,  always  at 
the  expense  of  the  loss  of  some  of  the  active  principles ; 
whereas,  with  the  use  of  a  suitable  knife  chopper,  the 
beans  can  be  and  should  be  reduced  to  a  fine  powder — 
the  finer  the  better  the  extraction,  minus  the  heat.  Too 
much  importance  cannot  be  attached  to  this  branch  of  the 
subject.  There  are  on  the  market  a  number  of  machines 
adapted  for  this  purpose,  and  they  can  be  had  in  either 
hand  or  belted  power  drives  from  $12.00  (the  American 
chopper,  hotel  size)  upward. 

EXHAUSTION  OF  THE  VANILLA  BEAN. 

EXTRACTION. 

The  process  for  the  rapid  and  thorough  exhaustion 
of  the  vanilla  bean  constitutes  the  principal  feature  in  the 
successful  operation  on  this  popular  and  costly  fruit, 
since  the  vanilla  bean  is  generally  conceded  as  ranking 
among  the  most  difficult  substances  from  which  to  ex- 
tract its  soluble  or  active  principles,  especially  by  perco- 
lation alone.  The  formula  to  be  fallowed  or  the  partic- 


1 8  Manufacture  of  Vanilla  Extracts 


ular  process  to  be  adopted  does  not  appear  to  be  of  such 
importance  as  that  the  complete  exhaustion  of  the  bean 
be  secured,  the  work  be  well  done,  whether  by  percola- 
tion, maceration,  digestion  or  a  combination  of  the  three. 
The  proper  menstruum,  of  course,  will  be  the  one 
that  intelligent  experiment  has  amply  demonstrated  as 
the  most  perfect  in  exhausting  and  preserving  the  im- 
portant principles.  Vanilla  extract  differs  from  most  of 
the  other  important  extracts  in  its  source,  being  made 
direct  from  the  aromatic  substance  in  its  crude  or  natural 
condition;  also  in  that  it  does  not  depend  on  a  volatile 
oil  for  its  virtue. 

PERCOLATION. 

Percolation  is  the  process  whereby  a  finely  divided 
fruit  or  drug  is  deprived  of  its  soluble  constituents  by 
the  descent  of  a  liquid  (menstruum)  through  it,  the  oper- 
ation also  embracing  the  process  of  straining  and  filtra- 
tion. Percolation  is  admirably  adapted  to  a  large  number 


Exhaustion  of  the  Vanilla  Bean  19 


of  drugs,  but  is  not  suitable  in  the  manufacture  of  vanilla 
extract,  for  the  following  reasons:  Slow  operation, 
which  must  not  exceed  fifty  drops  per  minute ;  excessive 
losses  in  alcoholic  evaporation,  ranging  from  10  to  15 
per  cent.;  incomplete  exhaustion  of  the  beans,  since  any 
irregular  particles  will  tend  to  form  an  heterogeneous 
mass,  offering  a  higher  resistance  to  the  flow  of  the 
menstruum  than  the  coarser  particles ;  and  the  beans, 
being  of  a  semi-soft  character,  when  placed  in  the  per- 
colator, have  the  tendency  of  conforming  into  packed 
masses  of  unequal  resistances,  resulting  in  the  flow  fol- 
lowing the  course  of  least  resistance,  with  the  consequent 
losses  from  incomplete  exhaustion.  See  Fig.  on  opposite 
page  (glass  percolator.) 

MACERATION. 

The  process  of  maceration  consists  of  exposing  the 
finely  reduced  beans  in  the  menstruum  until  they  are 
thoroughly  penetrated  and  the  soluble  or  active  princi- 
ples are  dissolved.  The  usual  method  is  to  introduce  the 
beans  into  an  air-tight  container ;  agitate  frequently  dur- 
ing four  to  six  months,  decant  the  clear  liquid;  express 
the  residue ;  filter  and  mix  the  liquids. 

According  to  Remington's  practice  of  pharmacy, 
"maceration  is  the  process  directed  by  the  German  Phar- 
macopoeia exclusively  in  preparing  tinctures,"  and  under 
the  heading  of  percolation,  he  adds :  "In  Great  Britain, 
France  and  Germany  the  process  (percolation)  is  well 
known  and  is  practiced  to  some  extent,  but  maceration 
still  holds  in  these  countries  the  chief  place  as  a  means 
of  extracting  the  soluble  principles  of  drugs";  further, 
"No  attempt  should  ever  be  made  to  produce  fluid  ex- 
tracts on  the  small  scale  without  previous  maceration," 
and  "the  intelligent  practice  of  the  process  of  percola- 


20  Manufacture  of  Vanilla  Extracts 


tion,  therefore,  requires  an  accurate  knowledge  of  the 
constituents  and  physical  properties  of  medicinal  sub- 
stances." 

DIGESTION. 

The  use  of  heat  for  extraction  is  an  old  and  dis- 
credited method  and  should  never  be  practiced,  since  the 
effect  of  heat  on  the  beans  has  the  tendency  of  decom- 
posing the  highly  flavored  aldehydes,  with  consequent 
loss  of  character. 

Exhausting  the  beans  in  vacuo  would  prove  practical 
were  it  not  for  the  fact  that  a  large  portion  of  the  vanillin 
ethers  and  esters  are  carried  over  into  the  pump,  which, 
of  course,  represents  an  irreparable  loss. 

The  most  rapid,  economical  and  thorough  process 
for  exhausting  the  active  principles  of  the  vanilla  bean 
consists  of  mechanical  maceration,  the  beans  and  mens- 
truum being  placed  in  a  suitable  machine  designed  for 
the  purpose  (see  figure  on  page  21).  This  machine  is 
fitted  with  an  air-tight  cover  for  receiving  and  discharg- 
ing the  content,  and  is  absolutely  air-tight,  thoroughly 
eliminating  all  possibility  of  alcoholic  evaporation.  The 
effect  of  the  violent,  protracted  surge  of  the  menstruum 
in  the  machine  is  to  force  it  through  the  cellular  structure 
of  the  beans  many  thousand  times  during  each  day's 
operation,  resulting  in  a  rapid  and  thorough  exhaustion 
by  the  combined  mechanical  and  solvent  power  of  the 
menstruum,  with  the  certainty  that  all  of  the  available 
vanillin,  resins  and  color  content  of  the  beans  are  in  solu- 
tion; whereas,  in  percolation,  the  menstruum  comes  in 
contact  with  the  beans  but  once. 

PERCOLATING  PROCESS. 

Select  a  percolator  (conical  preferred)  with  a  capa- 


Exhaustion  of  the  Vanilla  Bean 


21 


22  Manufacture  of  Vanilla  Extracts 

city  double  the  amount  required  to  hold  the  beans,  and 
place  at  the  bottom  a  small  quantity  of  washed  excelsior ; 
then  place  a  layer  of  beans  (cut  fine)  about  three  inches 
deep,  then  another  layer  of  excelsior,  then  another  of 
vanilla,  until  you  have  the  entire  quantity  of  the  beans 
in  the  percolator.  The  beans  should  be  packed,  using 
a  packing  stick  for  the  operation.  Considerable  care  and 
experience  are  required  so  that  the  packing  will  be  as 
uniform  as  possible  throughout  the  entire  mass.  Also 
guard  against  packing  too  tight,  since  in  that  event  the 
menstruum  will  refuse  to  flow;  on  the  other  hand,  un- 
less sufficient  resistance  is  offered  to  the  menstruum,  the 
net  results  will  be  far  from  satisfactory. 

Now  add  the  menstruum,  slowly,  until  the  beans  are 
covered ;  open  the  spigot,  and,  when  the  percolate  ap- 
pears, close  the  spigot,  and,  after  covering  the  percolator, 
allow  it  to  stand  twenty-four  hours  to  macerate;  then 
open  the  spigot  and  permit  the  percolate  to  proceed,  add- 
ing the  menstruum  until  completed,  which  should  be  in 
from  four  to  five  days. 

Place  the  dregs  into  a  cotton  bag,  put  into  a  power- 
ful screw  press  and  express,  filter  and  add  to  the  perco- 
late ;  next  add  the  sugar,  completing  the  operation.  The 
dregs  should  be  saved  for  making  a  second  quality  of 
extract,  but  the  resultant  liquid  would  not  pass  as  a  legal 
vanilla  and  would  have  to  be  labeled  "imitation." 

MECHANICAL   MACERATION-PROCESS. 

Place  the  menstruum  into  the  container  of  the  ma- 
chine; next,  add  the  finely  cut  (not  ground)  beans,  screw 
down  the  air-tight  cover  and  start  the  machine.  From 
two  to  three  days  are  sufficient  to  complete  the  exhaus- 
tion, since  the  beans  and  menstruum  are  brought  into  a 
surging  contact,  26,000  times  per  day. 


Formula  for  Making  Vanilla  Extract  23 

The  entire  mass  can  now  be  transferred  to  a  perco- 
lator for  clarifying,  although  the  use  of  the  double  pres- 
sure filter  and  percolator,  described  on  page  21,  will  be 
found  the  most  rapid  and  satisfactory.  After  the  extract 
has  ceased  to  flow  from  the  dregs,  ascertain  the  amount 
necessary  for  completing  the  volume  of  finished  product 
and  add  that  amount  of  water  in  the  filter  (water  dis- 
placement) ;  pour  the  water  very  carefully,  letting  it  fall 
on  a  glass  plate  so  that  the  position  of  the  beans  may 
not  be  disturbed.  If  you  use  sugar  in  your  vanilla,  do 
not  fail  to  allow  for  the  volume  increase  (see  sugar  table 
page  71).  Always  add  the  sugar  to  the  finished  product. 

We  will  suppose  that  the  batch  completed  represented 
25  gallons,  and  that  the  menstruum  used  is  what  is  known 
as  dilute  alcohol,  viz.,  equal  parts  by  volume;  next  add 
sufficient  water  in  the  filter  until  i2l/2  gallons  of  water 
washings  has  been  obtained.  The  use  of  this  water  will 
be  found  under  the  heading  of  menstruum  (solvent). 

FORMULA. 

The  Federal  "Standards  of  Purity  for  Food  Prod- 
ucts" defines  vanilla  extract  as  follows : 

Vanilla  extract  is  the  flavoring  extract  pre- 
pared from  vanilla  bean,  with  or  without  sugar 
or  glycerin,  and  contains  in  one  hundred  (100) 
cubic  centimeters  the  soluble  matters  from  not 
less  than  ten  (10)  grams  of  the  vanilla  bean." 
"Vanilla  bean  is  the  dried,  cured  fruit  of 
Vanilla  planifolia,  Andrews." 

The  foot-note  on  page  13  of  Circular  No.  19,  issued 
by  the  Department  of  Agriculture,  contains  the  follow- 
ing: 

"The  flavoring  extracts  herein  described  are 
intended  solely  for  food  purposes  and  are  not 


24  Manufacture  of  Vanilla  Extracts 

to  be  confounded  with  similar  preparations  de- 
scribed in  the  Pharmacopoeia  for  medicinal  pur- 
poses." 

Since  10  per  cent.,  or  12  4/5  ounces,  of  beans  to  the 
gallon  is  the  minimum  allowed  by  law,  the  necessity  of 
extracting  all  of  the  soluble  principles  is  at  once  appar- 
ent. However,  as  a  matter  of  precaution,  it  is  much  more 
advisable  to  employ  13  or  14  ounces  to  the  gallon,  as  per 
the  following  formula: 

Vanilla  beans,  cut  very  fine. . . .    14  ounces 
Cologne  spirits  (190  proof)  ....    ^  gallon 

Pure  water y2  gallon 

Cane  sugar  to  suit  (5  to  10  per  cent.). 
(Sugar  vs.  Glycerin.) 

The  philosophy  of  adding  glycerin  to  vanilla  was 
based  on  the  theory  that  glycerin  acts  as  a  binder  during 
baking  operations.  While  it  is  true  that  vanillin  is  sol- 
uble in  glycerin,  and  glycerin  is  a  non-volatile  or  fixed 
body,  various  baking  tests  failed  to  substantiate  the  the- 
ory. The  use  of  glycerin  has  many  supporters,  while 
others,  including  such  eminent  authorities  as  Dr.  C.  P. 
Nicholls  ("Monograph  on  Flavoring  Extracts,"  by  Har- 
rop),  writes  as  follows:  "A  mixture  of  cologne  spirits, 
water  and  glycerin  has  been  tried,  but  I  have  not  found 
the  addition  of  glycerin  an  improvement." 

The  use  of  sugar  is  to  be  recommended,  since  it  will 
increase  the  body  and  help  to  bring  out  the  flavor. 

AGEING. 

The  principal  virtue  in  storing  vanilla  in  wood  for  a 
long  period  consists  of  dealcoholization.  This  can  be 
demonstrated  by  dealcoholizing  a  sample  in  an  evaporat- 
ing dish  at  room  temperature,  and  comparing  with  sample 


Manufacture  of  Tonka  Extract  25 

not  so  treated.  Ageing  practically  amounts  to  concen- 
trating, since  alcohol  is  not  an  active  principle,  and  al- 
though at  least  50  per  cent,  by  volume  of  alcohol  is  neces- 
sary to  extract  the  vanillin,  resins  and  other  active  prin- 
ciples after  once  being  dissolved,  they  will  remain  in  solu- 
tion even  when  the  alcolohic  content  of  the  extract  has 
been  reduced  15  per  cent. 

The  lowering  of  the  alcoholic  strength  by  the  direct 
addition  of  water  will  precipitate  the  greater  portion  of 
the  resins,  and  resins  once  thrown  out  of  solution  in  this 
manner  do  not  dissolve  again  by  simply  adding  a  little 
more  alcohol. 

TONKA  EXTRACT. 

"Tonka  extract  is  the  flavoring  extract  pre- 
pared from  tonka  bean,  with  or  without  sugar 
or  glycerin,  and  contains  not  less  than  one-tenth 
(o.i)  per  cent,  by  weight  of  coumarin  extracted 
from  the  tonka  bean,  together  with  a  corre- 
sponding proportion  of  the  other  soluble  matters 
thereof." 

The  tonka  bean  is  the  odoriferous  seed  of  Wilding- 
ham  (Dipteryx  odorata),  a  large  tree  growing  in  Guiana. 
Two  varieties  commonly  found  in  the  market  are  Angos- 
tura and  Para,  the  former  being  held  at  a  much  higher 
price  than  the  latter.  Another  kind,  Surinam,  is  also 
known  to  the  trade. 

The  active  or  odorous  principle  of  the  tonka  bean 
consists  chiefly  of  coumarin,  a  rhomboidal,  somewhat 
irregular  crystalline  compound  (C9H8O2),  the  anhydride 
of  coumaric  acid.  It  is  prepared  synthetically  from  sweet 
clover,  melilot,  and  other  plants.  The  tonka  bean  has  a 
strong,  agreeable,  rather  heavy,  aromatic  odor  which, 
while  not  resembling  the  vanilla  in  flavor,  is  sometimes 


26  Manufacture  of  Imitation  Vanilla  Extracts 


used  to  "strengthen"  vanilla,  the  proportion  in  which  it 
may  be  mixed  with  vanilla  being  a  matter  of  taste  and 
cost. 

IMITATION  VANILLA. 

The  principal  ingredients  employed  in  the  manufac- 
ture of  imitation  vanilla  are  synthetic  vanillin  and  cou- 
marin.  The  characteristic  features  of  coumarin  is  de- 
scribed under  heading  of  "Tonka  Extract."  Synthetic 
vanillin  is  obtained  from  eugenol,  the  heavy  oil  of  clove. 
The  natural  vanillin  and  the  synthetic  vanillin  are  chemi- 
cally identical,  but  in  the  flavoring  there  is  a  perceptible 
difference  in  favor  of  the  natural.  However,  it  is  rather 
difficult  to  explain  how  and  where  the  difference  exists. 
Vanillin  alone  is  too  delicate  for  general  results,  and  a 
slight  proportion  of  coumarin  is  necessary  to  bring  out 
its  qualities,  as  per  the  following  formula : 

Vanillin   7  ounces 

Coumarin I  ounce 

Cane  sugar 8  pounds 

Spirits    3  gallons 

Pure  water  to  make 10  gallons 

Caramel  color  to  suit. 

Dissolve  the  vanillin  and  coumarin  in  the  alcohol;  next 
dissolve  the  sugar  in  the  water  and  mix ;  filter,  if  neces- 
sary. 

A  proportion  of  one  part  coumarin  to  four  parts 
vanillin  may  perhaps  please  some  customers,  particularly 
for  culinary  purposes.  A  product  of  this  character  will 
be  found  much  stronger  and  considerably  cheaper,  but 
of  course  it  lacks  the  delicate  character : 

Vanillin    4  ounces 

Coumarin    I  ounce 

Cane  sugar  6  pounds 


Manufacture  of  Non-Alcoholic  Extracts  27 

Spirits   YZ  gallon 

Pure  water  to  make 7  gallons 

Caramel  color  to  suit. 
Proceed  as  in  first  formula. 

WHITE   VANILLA. 

There  will  be  found  an  occasional  demand  for  a 
"white  vanilla."  All  that  is  necessary  is  to  eliminate  the 
color  from  the  foregoing  formulas.  The  only  advantage 
it  possesses  is  the  absence  of  any  tint  when  used  in  white 
work  such  as  frostings,  etc.  It  should  be  protected  from 
strong  light  owing  to  its  tendency  to  discolor. 

USES    HOT   AND   COLD. 

Tests  on  syrups,  cold  custards,  ice  cream,  cake  and 
candy  have  amply  demonstrated  the  relative  value  of 
true  and  synthetic  flavors  for  usage  in  hot  or  cold  work. 
On  all  cold  work,  the  true  flavor  showed  a  distinct  ad- 
vantage, while  on  hot  work  the  synthetic  proved  the  more 
lasting  and  valuable.  This  rule  holds  good  with  all 
flavors ;  the  vanilla  lost  most  of  its  highly  flavored  esters 
by  the  action  of  heat,  while  vanillin  seemed  to  hold  its 
full  power. 

NON-ALCOHOLIC  EXTRACTS. 

Non-alcoholic  flavors  are  prepared  in  two  forms,  viz. : 
Powder  and  paste.  In  the  powder  form  the  composition 
is  usually  the  essential  oil  incorporated  with  cane  sugar 
and  glycerine  in  about  the  following  proportions : 

Granulated  cane  sugar 65  pounds 

Oil  of  bitter  almonds 3  pounds 

Glycerin,  C.  P 2  pounds 

The  ingredients  are  thoroughly  mixed  and  packed  in 
paper-lined  air-tight  tin  containers. 

In  the  paste  form,  the  composition  and  proportions 
are  about  as  follows: 


28  Manufacture  of  Non-Alcoholic  Extracts 

Vanillin   2  ounces 

Coumarin   J/2  ounce 

Glycerin,  a  sufficient  quantity. 
Caramel  color,  a  sufficient  quantity. 

Glucose,  quantity  sufficient  to  make  14  pints. 
The  vanillin  and  coumarin  are  thoroughly  mixed  with  a 
sufficient  quantity  of  glycerin  until  a  smooth  paste  re- 
sults, then  add  the  glucose,  thoroughly  mix,  and  lastly 
add  the  caramel  color  to  the  desired  shade.  These  goods 
are  packed  in  one  and  two-ounce  collapsible  tubes. 

The  legal  requirements  having  reference  to  the  proper 
labeling  of  these  preparations  should  be  very  carefully 
investigated  before  attempting  to  place  them  on  the  mar- 
ket, since  they  are  not  entitled  to  the  term  "flavoring  ex- 
tracts," the  Department  of  Agriculture  specifying  an 
extract  as  a  solution  in  ethyl  alcohol. 

MENSTRUUM. 

The  subject,  alcohol  content  of  menstruums,  is  of  vital 
interest  for  the  following  reasons : 

First — Since  alcohol  does  not  contribute  to  the  flavor- 
ing value  of  any  extract,  being  entirely  dissipated  when 
used  in  baking,  the  per  cent,  necessary  is  the  amount 
that  will  thoroughly  extract  the  available  active  princi- 
ples and  preserve  them  at  the  lowest  temperature  to 
which  the  extracts  will  be  exposed  after  shipping;  hence 
any  surplus  quantity  employed  will  represent  an  actual 
waste. 

Second — Vanilla  being  regarded  as  one  of  the  most 
delicate  flavors  known,  it  is  always  desirable  to  put  the 
finished  product  on  the  market  with  the  lowest  per  cent, 
of  alcohol  possible,  conditional  that  all  of  the  available 
vanillin  and  resins  have  been  extracted  and  held  in  solu- 
tion. The  minimum  per  cent,  is  thirty,  since  in  the  event 


Alcoholic  Content  of  Menstruums  29 

of  the  alcohol  falling  below  this  number,  the  Government 
chemists  invariably  go  further  and  test  for  total  solids. 

Third — No  manufacturer  would  knowingly  add  an 
unnecessary  cost  to  any  of  his  products. 

The  most  intelligent  method  for  determining  the  per 
cent,  of  alcohol  necessary  is  to  prepare  small  test  batches, 
using,  as  a  minimum,  45  and  proceeding  up  to  55  per 
cent,  by  volume.  Fifty  per  cent,  as  a  rule  is  ample  with 
the  average  beans,  and  occasionally  we  find  old  crop  dry 
Mexicans  that  will  operate  nicely  on  45  and  40  per  cent. 
The  principal  trouble  to  guard  against  is  the  question  of 
clarification,  due  to  the  fact  that  all  vanilla  beans  con- 
tain a  mucilaginous  (gummy)  product.  As  this  matter 
is  insoluble  in  strong  alcohol,  it  is  necessary  to  employ 
sufficient  alcohol  to  keep  the  gummy  matter  out  of  solu- 
tion. To  overcome  the  necessity  of  employing  a  high 
per  cent,  of  alcohol  (above  50  by  volume),  several  proc- 
esses have  been  tried  out  with  more  or  less  success. 

First — By  the  removal  of  the  mucilaginous  principle 
with  the  use  of  boiling  water.  While  this  method  cer- 
tainly does  remove  the  gum,  it  also  has  the  effect  of  de- 
composing some  of  the  more  volatile  aldehydes  and 
esters;  there  is  also  the  loss  by  vaporizing  of  some  of 
the  vanillin.  If  the  water  used  for  this  purpose  was  not 
used  in  the  making  up  of  the  menstruum,  there  would 
be  quite  a  loss  of  vanillin,  since  this  product  is  soluble 
in  hot  water. 

Second — By  drying  the  beans  after  cutting,  the  beans 
being  spread  out  in  a  thin  layer  and  exposed  to  a  tem- 
perature of  not  more  than  no  degrees  F.  The  process, 
if  properly  conducted,  will  harden  the  gum  and  in  conse- 
quence permit  the  use  of  a  weaker  menstruum.  It  must 
not  be  forgotten  that  the  effect  of  the  heat  on  the  beans 
has  the  tendency  of  vaporizing  some  of  the  more  volatile 


30  Alcoholic  Content  of  Menstruums 

constituents  of  the  bean,  with  the  consequent  deteriora- 
tion of  the  finished  product. 

Third — By  the  use  of  a  strong  primary  menstruum, 
as  follows : 

Vanilla  beans,  finely  cut I  pound 

Cane  sugar   i  pound 

Alcohol,  190  proof 5  pints 

Pure  water   3  pints 

The  alcohol  and  water  must  be  mixed  previous  to  pour- 
ing on  the  beans,  this  rule  holding  good  in  any  process 
followed. 

The  above  produces  an  extract  in  the  proportion  of 
one  part  of  beans  to  eight  parts  of  extract.  By  adding 
two  pints  of  water  to  each  eight  pints  of  finished  ex- 
tract, you  produce  an  extract  in  the  proportion  of  one  to 
ten,  conforming  with  the  National  Food  Laws,  as  well 
as  all  the  State  laws.  The  extra  water  is  added  after 
removing  the  extract  from  the  beans  and  after  the  extract 
has  stood  a  few  days. 

There  is  one  serious  objection  to  this  process  in  that 
it  is  impossible  to  add  water  to  a  finished  extract  with- 
out throwing  out  of  solution  a  perceptible  amount  of  the 
resin  content;  and  since  it  is  these  resins  that  serve  as 
an  index  to  the  analytical  chemist  in  determining  whether 
10  per  cent,  of  beans  was  used,  the  process  is  not  recom- 
mended. 

Fourth — By  the  use  of  "water-washings"  described 
under  "Mechanical  Maceration."  The  process  produces 
the  best  results  of  all  methods  heretofore  described  and 
operates  under  the  following  principle :  When  the  ex- 
hausted beans  are  treated  with  water,  the  resultant  prod- 
uct is  known  as  water- washings ;  and  since  these  gums 
are  insoluble  in  alcohol  and  are  freely  soluble  in  water, 
the  water-washings  contain  a  very  appreciable  amount 


Testing  Vanilla  Extracts  31 

of  the  gum  in  solution ;  and  when  about  an  equal  amount 
of  alcohol  is  added,  the  mucilage  is  thrown  out  of  solu- 
tion (precipitation)  and  gradually  settles  to  the  bottom. 
In  practice,  the  beans  are  placed  in  the  container  and  the 
alcohol  and  water  washings  are  mixed  and  added  to  the 
beans  in  the  least  possible  time  required.  If,  under  ordi- 
nary conditions,  the  gum  is  dissolved  with  the  use  of  the 
water-washings,  the  gum  from  the  beans  would  unite 
with  the  gum  thrown  out  of  solution  from  the  washings 
and  both  would  settle  to  the  bottom  at  one  and  the  same 
time.  This  operation  requires  the  least  time  and  labor, 
while  no  loss  of  any  of  the  active  principles  is  possible. 

Other  conditions  being  equal,  well  cured  old  crop 
beans  are  always  to  be  preferred,  for  as  a  general  rule 
they  will  produce  a  clear  extract  with  a  much  less 
amount  of  alcohol. 

CARE  OF  FINISHED  EXTRACTS. 

Finished  extracts  should  be  well  protected  from  the 
decomposing  chemical  action  of  strong  light,  for  if  this 
is  not  heeded  the  extracts  will  eventually  be  ruined. 

DEMONSTRATION. 

The  old  habit  of  testing  extracts,  particularly  vanilla, 
by  eliminating  the  alcohol  by  way  of  friction  between  the 
hands,  is  decidedly  impractical,  since  by  this  method  the 
exudation  from  the  pores  of  the  skin  of  the  hands  adds 
an  odor  to  the  vanilla  that  certainly  does  not  tend  to  im- 
prove it.  The  most  satisfactory  method  is  with  the  use 
of  an  atomizer,  which  should  be  operated  up  to  within 
about  three  feet  of  the  prospective  buyer.  The  results 
in  a  demonstrative  way  are  all  that  could  be  desired,  as 
when  vanilla  is  finely  subdivided  the  alcohol  seems  to  be 
entirely  eliminated  while  traveling  through  space,  and 
the  buyer  gets  the  full  benefit  of  the  vanilla  character. 


32  Manufacture  of  Lemon  Extracts 


LEMON  EXTRACTS 


LEMON  EXTRACT. 

The  flavoring  preparation  next  in  importance  to 
vanilla  is  lemon  extract.  The  Federal  ''Standards  of 
Purity  for  Food  Products"  Circular  No.  19  defines  lemon 
extract  as  follows: 

"Lemon  extract  is  the  flavoring  extract  pre- 
pared from  oil  of  lemon,  or  from  lemon  peel,  or 
both,  and  contains  not  less  than  five  (5)  per 
cent,  by  volume  of  oil  of  lemon"; 

and  further, 

"Oil  of  lemon  is  the  volatile  oil  obtained,  by 
expression  or  alcoholic  solution,  from  the  fresh 
peel  of  the  lemon  (Citrus  limonum  L.),  has  an 
optical  rotation  (25°  C.)  of  not  less  than  +60° 
in  a  loo-millimeter  tube,  and  contains  not  less 
than  four  (4)  per  cent,  by  weight  of  citral." 

Lemon  oil  is  a  veiy  complex  body,  consisting  of  at 
least  15  constituents.  Of  these  the  terpenes  compose 
about  90  per  cent,  of  the  oil,  serving  mainly  as  a  vehicle 
for  the  essential  ingredients,  viz.:  the  aldehydes,  includ- 
ing citral,  4  to  6  per  cent.,  the  alcohols  and  esters  and 
other  compounds  4  to  \S  per  cent.  The  entire  oil  is  read- 
ily soluble  in  strong  akohol  (80  per  cent,  or  more)  which 
constitutes  the  most  expensive  ingredient,  since  its  cost 
is  a  trifle  over  75  per  c»nt.  of  the  total  cost  of  the  extract. 
Citral  is  the  chief  esseitial  ingredient,  but  citral  alone  is 
not  lemon,  the  remaining  ingredients  being  necessary  to 
fully  develop  the  true  lemon  character. 


Oil  of  Lemon  33 


The  terpenes  are  very  prone  to  decomposition ;  ex- 
posed to  the  action  of  light  and  heat  with  access  of  air, 
they  quickly  develop  an  odor  and  taste  of  turpentine. 

Oil  of  lemon  should  be  kept  in  well  stoppered  con- 
tainers, in  a  cool  place,  protected  from  the  chemical  ac- 
tion of  light.  The  contents  of  an  original  package,  after 
having  a  portion  removed,  can  be  kept  in  a  fragrant 
condition  by  adding  to  each  pound  of  oil  one  ounce  of 
alcohol ;  shake  well,  and  next  add  one  ounce  of  water 
and  again  shake.  The  water  withdraws  the  alcohol  from 
the  oil  and  collects  as  dilute  alcohol  at  the  bottom  of  the 
container,  where  it  should  be  permitted  to  remain  until 
the  oil  has  been  used,  shaking  each  time  the  container  has 
been  opened.  Oil  of  lemon  so  treated  has  been  kept  fresh 
and  fragrant  for  fourteen  months. 

Oil  of  orange  may  be  treated  in  a  similar  manner 
with  excellent  results. 

Oil  of  lemon  can  be  kept  for  an  indefinite  period  un- 
der the  most  unfavorable  conditions  known  if  from  I  to 
2  per  cent,  of  a  fixed  oil  is  incorporated  with  it.  Such 
oils  as  cotton  and  olive  are  well  adapted  for  this  purpose. 
A  test  sample  treated  in  this  manner  has  been  exposed 
to  the  action  of  heat  and  light  for  two  years,  and  at  the 
end  of  that  time  did  not  indicate  any  deterioration  in  the 
least.  This  method  of  preserving  oil  is  well  adapted  to 
bakers'  and  confectioners'  use,  also  oils  intended  for  pre- 
paring terpeneless  extract  of  lemon ;  but  it  is  not  recom- 
mended for  use  in  whole  oil  lemon,  since  the  existence  of 
the  minute  quantities  of  the  fixed  oil  might  be  opposed 
by  the  pure  food  authorities. 

The  manufacture  of  extract  of  lemon  is  a  very  simple 
process,  the  formula  consisting  of  a  solution  of  5  per 
cent,  of  oil  of  lemon  in  strong  alcohol  as  per  the  fol- 
lowing : 


34  Manufacture  of  Lemon  Extracts 


Oil  of  lemon 6.4  ounces 

Grain  alcohol   121. 6  ounces 

128       ounces=i  gallon 
Mix  thoroughly,  let  stand  a  few  hours,  and  filter. 

Bear  in  mind  that  this  formula  contains  the  minimum 
allowed  by  the  food  laws,  and  the  author  would  suggest 
the  advisability  of  employing  a  larger  per  cent,  of  oil, 
since  there  is  always  a  liability  of  error  on  the  part  of 
the  manufacturer  or  analyst,  which  may  result  in  a  food 
law  case.  The  habit  of  obeying  the  law  in  the  letter, 
rather  than  in  the  spirit,  is  not  to  be  commended. 

That  this  position  has  been  adopted  by  some  of  the 
leading  manufacturers  is  attested  by  an  examination  of 
seven  of  the  most  popular  brands  on  the  market.  The 
per  cent,  of  whole  oil  of  lemon  varied  from  8  to  17  per 
cent.,  with  the  precipitation  and  centrifuge  method. 

TERPENELESS   EXTRACT   OF    LEMON. 

The  Federal  "Standards  of  Purity  for  Food  Prod- 
ucts" Circular  No.  19  defines  terpeneless  extract  of  lemon 
as  follows: 

"Terpeneless  extract  of  lemon  is  the  flavoring 
extract  prepared  by  shaking  oil  of  lemon  with 
dilute  alcohol,  or  by  dissolving  terpeneless  oil  of 
lemon  in  dilute  alcohol,  and  contains  not  less 
than  two-tenths  (0.2)  per  cent,  by  weight  of 
citral  derived  from  oil  of  lemon."  "Terpeneless 
oil  of  lemon  from  which  all  or  nearly  all  of  the 
terpenes  have  been  removed." 

Terpeneless  oil  of  lemon  is  simply  the  natural  oil  freed 
from  the  terpenes  by  distillation  under  vacuum.  These 
terpenes  are  bodies  or  chemical  compounds  which  con- 


Terpeneless  Extract  of  Lemon  35 


sist  entirely  of  hydrogen  and  carbon,  and  while  they  are 
considered  as  inert  and  worthless  as  a  flavoring  medium, 
they  require  a  strong  alcohol  for  solution.  Terpeneless 
oils  of  lemon  are  offered  by  the  trade  at  prices  ranging 
from  $20  to  $30  per  pound,  while  the  percentage  of  citral 
varies  from  between  40  to  65  per  cent.  The  lower  grade 
oils  have  been  freed  from  only  a  portion  of  the  terpenes 
and  will  not  dissolve  clear  in  a  50  per  cent,  by  volume  of 
a  190  proof  alcohol. 

The  words,  "nearly  all  of  the  terpenes  have  been  re- 
moved," no  doubt  account  for  the  presence  on  our  mar- 
kets of  oil  of  various  strengths  and  character.  When 
purchasing  a  terpeneless  lemon  oil,  the  most  logical 
method  for  the  manufacturer  to  pursue  would  be  as 
follows:  Purchase  a  high-grade  oil  of  a  reliable  house 
and  request  a  statement  in  the  form  of  a  guarantee,  hav- 
ing reference  to  the  citral  content,  which  should  like- 
wise appear  on  the  label ;  then,  and  then  only,  will  one  be 
able  to  intelligently  ascertain  the  amount  of  oil  required. 
The  amount  of  alcohol  required  should  be  sufficient  to 
dissolve  the  oil  (in  a  clear  state)  and  hold  it  in  solution 
at  the  lowest  winter  temperature  to  which  these  extracts 
would  be  subject  in  shipping  to  the  trade,  the  amount  in 
no  instance  being  less  than  50  per  cent,  by  volume  of  190 
proof. 

The  use  of  carbonate  of  magnesia  or  any  other  filter- 
ing medium  should  be  discouraged,  since  more  or  less  of 
the  citral  is  held  back  with  the  terpenes  and  magnesia, 
eliminating  the  element  of  certainty  in  computing  the  per 
cent,  of  citral  in  the  finished  product ;  while  with  the  use 
of  the  proper  oil,  no  filtering  is  necessary.  Whenever 
possible,  soft  or  distilled  water  should  be  used. 

The  advantages  of  terpeneless  extract  of  lemon  are 
as  follows :  They  will  not  develop  a  rancid  or  turpen- 


36  Manufacture  of  Lemon  Extracts 

tine  flavor  on  exposure  to  heat  or  strong  light,  because 
the  hydro-carbon — that  portion  of  the  oil  which  readily 
decomposes — is  not  present ;  and,  being  soluble  in  water, 
they  readily  mix  into  ices,  fountain  syrups,  etc.  There 
is  a  saving  of  about  50  per  cent,  of  alcohol,  and  they  can 
be  produced  at  the  lowest  possible  cost  for  the  strength, 
purity  and  permanence  of  flavor  obtained.  It  is  undoubt- 
edly true  that  this  class  of  products  is  useful  as  a  flavor- 
ing agent,  but,  as  is  true  of  all  such  products,  they  should 
be  labeled  exactly  what  they  are. 

MANUFACTURE    OF    TERPENELESS    LEMON    EXTRACT. 

Various  methods  have  been  employed  in  the  manufac- 
ture of  terpeneless  extract  of  lemon,  the  following  being 
among  the  most  popular : 

First — What  is  known  as  the  "shaking  out"  process 
consists  of  placing  the  oil  and  dilute  alcohol  into  an  air- 
tight container  and  churning  for  a  considerable  length 
of  time ;  then  allowing  the  mixture  to  stand  until  the  oily 
portion  rises  to  the  top,  when  the  lower  stratum  is  drawn 
off  and  filtered  with  the  aid  of  magnesium  carbonate  or 
kieselguhr  (an  infusorial  earth)  to  remove  globules  of 
oil  held  in  suspension.  The  degree  of  citral  removed 
depends,  first,  upon  the  alcoholic  strength,  and  second, 
upon  the  thoroughness  of  the  agitation,  facilitating  the 
extracting  alcohol  to  come  into  close  contact  with  the 
very  minute  globules  of  whole  oil  of  lemon.  The  oily 
residue  is  generally  subjected  to  a  second  churning  proc- 
ess, in  an  effort  to  remove  the  entire  amount  of  the  deli- 
cate flavoring  constituent,  viz. :  citral,  which  is  the  prin- 
cipal flavoring  ingredient  in  oil  of  lemon. 

Second — Place  the  lemon  oil  and  alcohol  into  a  suit- 
able container  (an  alcohol  barrel  free  from  glue)  and 


Tcrpeneless  Lemon  Extracts  37 


agitate  occasionally  during  a  period  of  twenty- four 
hours;  next  add  magnesium  carbonate  or  kieselguhr 
(about  24  ounce  to  each  gallon),  shake  thoroughly  and 
add  the  water  lukewarm,  shaking  thoroughly  after  each 
gallon  addition,  and,  when  complete,  agitate  or  churn 
for  at  least  one  day;  next  place  the  barrel  on  a  rack 
and  allow  the  filtering  medium  to  subside;  next  syphon 
off  the  almost  clear  liquid,  being  careful  not  to  insert 
the  hose  too  close  to  the  filtering  medium  at  the  bottom 
of  the  barrel.  In  this  manner  the  filtering  operation  will 
operate  quite  rapidly.  Lastly,  place  the  remaining  por- 
tion of  the  mixture  into  the  filter,  using  either  heavy 
white  paper  or  felt.  A  great  deal  of  conscientious  care 
and  good  judgment  must  be  exercised  in  this  process; 
otherwise  a  considerable  waste  of  materials  will  result. 
The  filtering  medium  will,  in  both  cases,  be  found  to  con- 
tain the  terpene  product,  together  with  considerable  of 
the  extract,  and  this  can  be  recovered  by  placing  the  me- 
dium into  a  close-mesh  cotton  or  linen  bag  and  then  put- 
ting the  bag  into  a  powerful  screw  press  to  express  the 
products.  Two  distinctive  layers  will  result;  the  lower, 
which  is  the  extract  and  which  can  be  syphoned  off,  and 
the  upper,  the  objectionable  terpene  principle. 

The  basis  for  computing  the  strength  of  a  lemon  ex- 
tract lies  in  the  percentage  of  the  citral  it  contains.  An 
extract  made  from  the  whole  oil  will  contain  about  .2  per 
cent,  of  citral  in  the  finished  extract,  provided  that  5  per 
cent,  of  oil  has  been  used.  Lemon  oil  usually  contains 
about  4  per  cent,  of  citral ;  therefore,  in  the  finished  ex- 
tract there  will  be  .O5X.O4=.OO2,  or  .2  per  cent.  Theo- 
retically, 5  per  cent,  of  whole  lemon  oil,  containing  4  per 
cent,  of  citral,  should  yield  the  required  .2  per  cent,  of 
citral  to  a  terpeneless  lemon  extract  made  by  the  shaking- 
out  process.  In  practice,  this  is  far  from  being  correct, 


38  Manufacture  of  Lemon  Extracts 

due  mainly  to  the  fact  that  more  or  less  of  the  citral  is 
withheld  in  the  terpenes  and  filtering  medium.  The 
safest  course  to  pursue  would  be  the  employment  of  at 
least  8  per  cent,  of  oil  as  per  the  following  formula  : 

Spirits  190  proof  .............     59      ounces 

Water  (lukewarm)    ...........     59       ounces 

Oil,  lemon  ...................     10%  ounces 


Third  —  By  simply  dissolving  terpeneless  lemon  oil  in 
dilute  alcohol.  Processes  No.  i  and  No.  2  have  been  in 
use  many  years  and  are  still  quite  extensively  practiced. 
Practically  all  advantages  as  regards  certainty  of  citral 
content  and  cost  and  labor  are  in  favor  of  the  simple 
method  of  dissolving  terpeneless  lemon  oil  in  suitable 
strength  alcohol,  as  per  the  following  formula: 

Terpeneless  oil  of  lemon  (assaying 

66%  citral)    ..................  3^  drams 

Spirits  190  proof  ................  j£  gallon 

Water  (soft  preferred)   ..........  ^2  gallon 

Add  the  oil  to  the  spirits  and  shake  well;  next  add  the 
water,  gradually  shaking  after  each  addition;  then  filter 
through  paper,  if  necessary.  To  determine  the  citral 
content  in  the  finished  product,  proceed  as  follows: 

8  drams=i  ounce;  128  ounces= 

i  gallon,  or  .................    1024       drams 

add  to  the  above  the  oil  used.  .  .  .         3^  drams 


and  employ  the  total  as  the  divisor;  1027)  3.125  (.00304 
for  the  dividend  take  the  amount  of  oil  used;  the  quo- 
tient represents  the  per  cent,  of  oil  employed ;  next  mul- 
tiply the  per  cent,  of  oil  used  by  the  per  cent,  of  citral 
contained  in  the  oil : 


Terpeneless  Lemon  Extracts  39 


.304  representing  the  per  cent,  of  oil  used 

.66  representing  the  per  cent,  of  citral  con- 
tent  of  the  lemon  oil 


1824 
1824 


0.20064  representing  the  per  cent,  of  citral  in  the 
finished  product,  provided  that  no  filter- 
ing medium  has  been  employed. 

To  ascertain  the  amount  of  terpeneless  oil  required 
to  contain  the  necessary  2/10  per  cent,  citral  in  the  fin- 
ished product,  using  an  oil  assaying  60  per  cent,  citral, 
proceed  as  follows : 

Per  cent,  of  citral  in  the  oil  of  lemon 

is  the  divisor 60)  .002000  (.0034 

Per  cent,  of  citral  in  finished  prod- 
uct is  the  dividend 

Per  cent,  of  oil  required  is  the  quo- 
tient 

Number  of  drams  to  the  gallon     1024 

Times  per  cent,  of  oil  required   .0034 

3.4816  drams  to  the  gal. 

The  grated  exterior  rinds  of  fresh  yellow  lemons  are 
a  valuable  addition  to  any  lemon  extract,  adding  charac- 
ter and  piquancy,  in  fact,  all  that  could  be  desired  in  a 
high-grade  product. 

LEMON   FLAVOR — IMITATION. 

All  grades  of  lemon  extracts  below  the  standards 
specified  under  "Lemon  extract"  and  "Terpeneless  lemon 
extract"  must  be  labeled,  sold  and  invoiced  as  imita- 


40  Manufacture  of  Lemon  Flavor — Imitation 

tions.  All  products  labeled  and  sold  as  imitations  do  not 
require  a  specified  standard  of  purity  or  strength ;  hence, 
by  varying  the  proportions  of  formulas  submitted,  ex- 
tracts of  almost  any  desired  strength  and  cost  can  be 
made.  At  this  time,  the  Federal  and  most  State  laws 
permit  the  use  of  coloring,  provided  the  colors  used  are 
plainly  stated  on  the  label  and  are  of  the  "certified"  type. 
The  great  advantage  which  the  use  of  certified  colors  of- 
fers to  the  food  products  manufacturers  is  clearly  set 
forth  in  F.  I.  D.  (Food  Inspection  Decision)  No.  117, 
as  follows : 

"Food  Inspection  Decision  No.  76,  published 
July  13,  1907,  gives  a  list  of  seven  coal  tar  dyes 
which  may,  without  objection  from  the  Depart- 
ment of  Agriculture,  be  used  in  foods  until  fur- 
ther notice.  Food  Inspection  Decision  No.  77, 
published  September  25,  1907,  provides  for  the 
certification  of  dyes.  Certified  dyes  may  be  used 
in  foods  without  objection  by  the  Department 
of  Agriculture,  provided  the  use  of  the  dye  in 
food  does  not  conceal  damage  or  inferiority." 

Uncertified  coal  tar  dyes  are  likely  to  contain  arsenic 
and  other  poisonous  elements  which,  when  used  in  food, 
may  render  such  food  injurious  to  health,  and,  therefore, 
would  be  adulterated  under  the  law. 

The  active  principle  of  imitation  lemon  is  composed 
chiefly  of  citral  or  lemongrass.  One  ounce  of  citral  is 
equivalent  in  flavoring  power  to  one  pound  of  oil  of 
lemon,  but  is  decidedly  deficient  in  delicacy  and  charac- 
ter of  the  real  lemon  oil.  Commercial  citral  is  not  a  syn- 
thetic product,  its  common  source  being  lemongrass,  sepa- 
rated by  distillation.  The  per  cent,  of  citral  content  of 
lemongrass  varies  from  60  to  75  per  cent.  Citral  occu- 


Manufacture  of  Lemon  Flavor— Imitation  41 


pies  the  same  relation  to  lemon  flavor  as  coumarin  does 
to  vanilla,  but  it  does  not  blend  nearly  as  well.  In  the 
following  formulas  the  use  of  citral  or  lemongrass  are 
optional.  There  are  three  grades  of  lemongrass  on  the 
market,  viz. :  Native,  rectified  and  Java,  their  relative 
values  being  in  the  same  order : 

Terpeneless  oil  of  lemon ^2  dram 

Citral   y*  dram 

Oil  of  lemon 4  ounces 

Alcohol    3  pints 

Water  (lukewarm)    5  pints 

Magnesia — carbonate     2  ounces 

Dissolve  the  oils  in  the  alcohol,  mix  the  magnesia  and 
water,  and  add  slowly  together,  shaking  thoroughly  off 
and  on  for  one  day ;  filter  through  paper. 

Lemongrass     4  drams 

Alcohol    32  ounces 

Water  (lukewarm)    96  ounces 

Carbonate — Magnesia    I  ounce 

Treat  as  above. 

EXTRACT   OF   ORANGE. 

The  Federal  standard  of  extract  of  orange  and  ter- 
peneless  extract  of  orange  corresponds  in  all  respects  to 
lemon  extract.  As  in  the  case  of  the  lemon,  the  use  of 
the  grated  outer  rind  of  the  orange  is  a  valuable  addi- 
tion to  orange  extract.  There  are  no  substitutes  for 
orange  flavors,  the  cheapest  practical  formula  consisting 
of  the  terpeneless. 


42  Manufacture  of  Various  Extracts 


VARIOUS  EXTRACTS 


EXTRACT  OF  ALMOND. 

"Almond  extract  is  the  flavoring  extract  pre- 
pared from  oil  of  bitter  almonds,  free  from  hy- 
drocyanic acid,  and  contains  not  less  than  one 
(i)  per  cent,  by  volume  of  oil  of  bitter  al- 
monds." 

Oil  of  bitter  almonds,  commercial,  is  the  volatile  oil 
obtained  from  the  seed  of  the  bitter  almond  (Amygdalus 
communis  L.),  the  apricot  (Prunus  armenlaca  L.),  or  the 
peach  (Amygdalus  persica  L.). 

No.  i. 

Oil  of  almond 3  ounces 

Spirits    5  pints 

Water     3  pints 

Dissolve  the  oil  in  the  alcohol  and  add  water  gradually, 
shaking  after  each  addition;  filter  if  necessary. 

No.  2. 

Oil  of  almond i  3/10  ounces 

Spirits    52  ounces 

Water    76  ounces 

Proceed  as  in  formula  No.  i. 

A  very  satisfactory  imitation  can  be  prepared  by  the 
use  of  "Benzaldehyde,"  but,  like  all  other  synthetic 
flavors,  is  inferior  to  the  natural  product  when  used  in 
the  cold,  but  it  withstands  heat  better. 


Manufacture  of  Various  Extracts  43 

No.  3. 

Benzaldehyde    i%  ounces 

Spirits    45       ounces 

Water    83      ounces 

Proceed  as  above. 

WINTERGREEN   EXTRACT. 

"Wintergreen  extract  is  the  flavoring  extract 
prepared  from  oil  of  wintergreen,  and  contains 
not  less  than  three  (3)  per  cent,  by  volume  of 
oil  of  wintergreen."  "Oil  of  wintergreen  is  the 
volatile  oil  distilled  from  the  leaves  of  the  Gaul- 
theria  procumbens  L." 

No.  i. 

Oil  of  wintergreen 4  ounces 

Spirits    90  ounces 

Water     38  ounces 

Imitation  wintergreen  is  prepared  by  the  use  of  oil 
of  sweet  birch,  or  Methly  salicylate. 

No.  2. 
Oil    of    sweet    birch,    or    methyl 

salicylate    3^/2  ounces 

Spirits    76      ounces 

Water     52       ounces 

Mix,  and  filter  if  necessary. 

EXTRACT  OF  PEPPERMINT. 

"Peppermint  extract  is  the  flavoring  extract 
prepared  from  oil  of  peppermint,  or  from  pep- 
permint, or  both,  and  contains  not  less  than 
three  (3)  per  cent,  by  volume  of  oil  of  pepper- 
mint." "Oil  of  peppermint  is  the  volatile  oil 


44  Manufacture  of  Various  Extracts 

obtained  from  peppermint  and  contains  not  less 
than  fifty  (50)  per  cent,  by  weight  of  menthol." 

Substitutes  for  peppermint  of  a  practical  character 
are  not  known. 

No.  i. 

Oil  of  peppermint  4  ounces 

Spirits i  gallon 

Mix.  This  product  can  be  colored  with  the  use  of  pep- 
permint leaves  to  suit. 

In  the  event  of  a  cheaper  product  being  desired,  pre- 
pare a  terpeneless  extract  either  by  the  use  of  terpene- 
less  oil  of  peppermint  or  by  the  "shaking  out"  process,  as 
prescribed  for  terpeneless  extract  of  lemon.  Since  these 
products  fall  below  the  legal  standard,  they  should  be 
labeled,  sold  and  invoiced  as  an  imitation. 

EXTRACT   OF    GINGER. 

"Ginger  extract  is  the  flavoring  extract  pre- 
pared from  ginger  and  contains  in  each  one  hun- 
dred (100)  cubic  centimeters  the  alcohol-soluble 
matters  from  not  less  than  twenty  (20)  grams 
of  ginger." 

No.  i. 

Jamaica  ginger  (coarse  powder) 2  pounds 

Spirits i  gallon 

Place  the  ginger  in  a  narrow  percolator,  using  no  force 
in  packing,  always  providing  sufficient  washed-fine  ex- 
celsior in  the  apex  of  the  percolator  to  retain  the  ginger ; 
next  pour  on  the  alcohol,  and  when  the  entire  mass  is  sub- 
merged, cork  the  delivery  and  cover  the  top  and  let  stand 
for  several  days ;  then  percolate. 

Another  method,  in  the  absence  of  a  percolator,  is 
to  place  the  ginger  and  spirits  in  a  suitable  air-tight  con- 


Manufacture  of  Various  Extracts  45 

tainer,  such  as  a  packing  bottle  or  a  keg,  and  shake  fre- 
quently for  a  few  days ;  next  place  the  mass  on  a  coarse 
paper  filter  and  finish. 

Jamaica  ginger  is  always  to  be  preferred  to  any  of  the 
lower  grades,  since  the  character  is  not  only  the  finest, 
but  the  tendency  of  precipitates   (sediment)'  is  reduced 
to  a  minimum. 
No.  2. 

Oleo-resin  ginger  ( i  %  )   1 . 28  ounces 

Spirits    24  gallon 

Water  (soft)    }4  gallon 

Dissolve  the  oleo-resin  in  the  spirits  and  gradually  add 
the  water  lukewarm,  shaking  after  each  addition;  let 
stand  for  a  few  days ;  filter  through  paper,  using  a  small 
amount  of  precipitated  calcium  carbonate  as  a  medium  if 
necessary. 

For  a  cheaper  product  the  soluble  essence  is  recom- 
mended, as  follows: 
No.  3.   Soluble. 
Jamaica  ginger  (coarse  powder) ....   4  pounds 

Pumice  stone  (powdered)  4  ounces 

Lime  (slacked)    4  ounces 

Spirits  (dilute,  equal  parts)    I  gallon 

Rub  the  ginger  with  the  pumice  stone  and  lime  until 
thoroughly  mixed.  Moisten  with  the  dilute  alcohol  until 
saturated,  and  place  in  a  narrow  percolator,  being  care- 
ful not  to  use  force  in  packing,  simply  placing  it  in  to 
obtain  the  position  of  a  powder  to  be  percolated,  so  that 
the  menstruum  will  flow  through  uniformly.  Next  add 
the  dilute  alcohol  and  percolate  until  one  gallon  of  the 
percolate  is  obtained.  Let  stand  twenty-four  hours,  and 
filter  if  necessary.  The  pumice  should  be  repeatedly 
washed  in  water  prior  to  using. 


46  Manufacture  of  Various  Extracts 

No.  4.   Soluble. 

Fluid  extract  of  ginger  (U.  S.  P.)  . .  8  ounces 

Pumice,  powdered  and  washed  ....  2  ounces 

Water,  quantity  sufficient  to  make . .  24  ounces 

Pour  the  fluid  extract  of  ginger  into  a  bottle  and  add  the 
pumice,  shaking  thoroughly;  repeat  the  operation  for 
several  hours ;  next  add  the  water  in  the  proportion  of 
about  two  ounces  at  a  time,  shaking  after  each  addition. 
When  all  is  added,  repeat  the  agitation  occasionally  dur- 
ing twenty-four  hours,  then  filter,  returning  the  filtrate 
until  it  comes  through  clear,  and,  if  necessary,  add  suf- 
ficient water  to  produce  the  required  24  ounces  of  fin- 
ished product. 

EXTRACT    OF    ROSE. 

"Rose  extract  is  the  flavoring  extract  prepared 
from  otto  of  roses,  with  or  without  red  rose 
petals,  and  contains  not  less  than  four-tenths 
(0.4)  per  cent,  by  volume  of  otto  of  roses." 

Otto  of  roses  is  the  volatile  oil  obtained  from  the 
petals  of  Rosa  damascena  Mill.,  R.  moschata  Herrm. 

No.  i. 

Oil  of  rose  (otto)   y2  ounce 

Spirits   i  gallon 

Mix  and  filter  if  necessary. 

There  are  a  number  of  desirable  artificial  rose  oils 
on  the  market,  soluble  in  dilute  3  to  i  spirits,  suitable  for 
imitation  products,  costing  but  25  per  cent,  of  that  of  the 
genuine  oil.  To  increase  the  tone  or  piquancy  of  this 
product,  use  rose  geranium  of  the  very  best  quality,  as 
per  the  following: 


Manufacture  of  Various  Extracts  47 

No.  2. 

Oil  of  rose  (artificial)   2  drams 

Oil  rose  geranium  (best  quality)  ...    ]/?.  dram 

Oil  of  clove  (amboyna)   24  minims 

Spirits 3  quarts 

Water I  quart 

Filter  with  carbonate  of  magnesia  if  necessary.     Label 

an  imitation. 

EXTRACT    OF    ALLSPICE. 

The  Government  standards  do  not  include  allspice. 

Oil  of  allspice  (pimento)   2  drams 

Allspice  (coarse  powder)   3  ounces 

Spirits  (dilute)   2  pints 

Mix,  macerate  for  several  days,  and  filter. 

ANISE  EXTRACT. 

"Anise  extract  is  the  flavoring  extract  pre- 
pared from  oil  of  anise,  and  contains  not  less 
than  three  (3)  per  cent,  by  volume  of  oil  of 
anise." 

"Oil  of  anise  is  the  volatile  oil  obtained  from  the  anise 

seed." 

Oil  of  anise 4  ounces 

Spirits   I  gallon 

Mix  and  filter  if  necessary. 

CELERY  EXTRACT. 

"Celery  seed  extract  is  the  flavoring  extract 
prepared  from  celery  seed  or  the  oil  of  celery 
seed,  or  both,  and  contains  not  less  than  three- 
tenths  (0.3)  per  cent,  by  volume  of  oil  of  celery 
seed." 


48  Manufacture  of  Various  Extracts 

"Oil  of  celery  seed  is  the  volatile  oil  obtained  from 
celery  seed." 

Oil  of  celery  seed 3^  drams 

Spirits     3       quarts 

Water i       quart 

Mix  and  filter  if  necessary. 

EXTRACT  OF  CINNAMON. 

"Cinnamon  extract  is  the  flavoring  extract 
prepared  from  oil  of  cinnamon,  and  contains 
not  less  than  two  (2)  per  cent,  by  volume  of  oil 
of  cinnamon." 

"Oil  of  cinnamon  is  the  lead-free  volatile  oil  obtained 
from  the  bark  of  the  Ceylon  cinnamon  (Cinnamomum 
zeylanicum  Breyne),  and  contains  not  less  than  sixty- 
five  (65)  per  cent,  by  weight  of  cinnamic  aldehyde  and 
not  more  than  ten  (10)  per  cent,  by  weight  of  eugenol." 

Oil  of  cinnamon 2 . 56  ounces 

Spirits    • 90        ounces 

Water 38        ounces 

Thoroughly  shake  the  oil  with  the  alcohol  and  add  the 
water  gradually,  shaking  after  each  addition;  filter  if 
necessary. 

The  standard  for  cassia  extract  is  the  same  as  that 
for  cinnamon,  but  the  oil  specification  is  somewhat  dif- 
ferent, as  follows : 

"Oil  of  cassia  is  the  lead-free  volatile  oil  ob- 
tained from  the  leaves  or  bark  of  the  Cina- 
momum  cassia  BL,  and  contains  not  less  than 
seventy-five  (75)  per  cent,  by  weight  of  cin- 
namic aldehyde." 


Manufacture  of  Various  Extracts  49 


EXTRACT  OF  CLOVES. 

"Clove  extract  is  the  flavoring  extract  pre- 
pared from  oil  of  cloves,  and  contains  not  less 
than  two    (2)    per  cent,   by  volume  of  oil  of 
cloves." 
Formula  is  the  same  as  that  for  cinnamon  extract. 

EXTRACT  OF   MINT    (SPEARMINT). 

"Spearmint  extract  is  the  flavoring  extract 
prepared  from  oil  of  spearmint,  or  from  spear- 
mint, or  both,  and  contains  not  less  than  three 
(3)  Per  cent,  by  volume  of  oil  of  spearmint." 
Formula  same  as  for  anise  extract. 

EXTRACT  OF  CHOCOLATE. 

(No  Government  Standard.) 

Curacao  cocoa  i  J/2  pounds 

Dilute  spirits  (equal  parts)    I       gallon 

Mix  thoroughly  and  macerate  for  from  five  to  ten  days, 
shaking  occasionally,  and  filter  or  percolate ;  addition  of 
extract  of  vanilla  is  an  improvement. 

EXTRACT   SARSAPARILLA — SOLUBLE — AN   IMITATION. 

Oil  of  wintergreen I  ounce 

Oil  of  sassafras  */2  ounce 

Oil  of  cassia  (or  cinnamon) I  dram 

Oil  of  fennel I  dram 

Oil  of  caraway I  dram 

Oil  of  anise 4  drams 

Alcohol  and  water  of  each y2  gallon 

Caramel  color  to  suit. 


50  Ethereal  Imitation  Flavors 

Dissolve  the  various  oils  in  the  alcohol  and  rub  with  three 
ounces  of  carbonate  of  magnesia  in  a  mortar.  Transfer 
the  mixture  into  a  bottle  and  add  the  water,  shaking  after 
each  addition ;  allow  to  macerate  for  a  few  days,  and  ni- 
ter through  paper,  adding  sufficient  water  through  the 
paper  to  make  one  gallon. 

EXTRACT  PISTACHIO  IMITATION. 
NO.   I. 

Extract  of  almond 2  ounces 

Extract  of  vanilla 4  ounces 

Oil  of  neroli I  drop 

Mix. 

No.  2. 

Oil  of  orange 4  drams 

Oil  of  cassia  or  cinnamon i  dram 

Oil  of  nutmeg 1^2  drams 

Oil  of  bitter  almonds 15  minims 

Oil  of  calamus 15  minims 

Oil  of  cloves   30  minims 

Spirits   12  ounces 

Water   4  ounces 

Magnesia,  carbonate 3       drams 

Dissolve  the  various  oils  in  the  alcohol  and  rub  with  the 
magnesia;  add  the  water  with  agitation;  let  stand  a  few 
hours,  and  filter. 

ETHEREAL  IMITATION   FLAVORS. 

Such  flavors  as  pineapple,  strawberry,  banana,  rasp- 
berry, cherry,  etc.,  are  prepared  from  concentrated  fruit 
ethers.  Owing  to  the  large  number  of  individual  ethers 
required  to  compound  the  various  flavors,  considering  the 


Ethereal  Imitation  Flavors  51 

small  demand  in  general  and  the  variations  of  formula, 
it  is  more  economical,  as  well  as  more  satisfactory,  to 
purchase  from  a  reliable  essential  oil  house  the  mixed 
ethers  representing  the  flavors  desired.  These  ethers 
were  formerly  known  as  "Fruit  Oils/'  but  under  the 
Federal  Food  and  Drugs  Act  this  term  has  gone  into 
disuse. 

As  to  the  status  of  these  ethereal  flavors  under  the 
food  laws,  there  is  pending  at  present  under  the  Penn- 
sylvania State  law  litigation  as  to  whether  Amyl  Acetate 
and,  possibly,  one  or  two  other  ethers  may  be  used  in 
food  products.  Undoubtedly  the  general  disposition  of 
food  officials  is  against  such  substitute  materials.  They 
have  never  been  very  popular,  but  certain  sections  of  the 
country  enjoy  a  fair  demand.  It  is  necessary  so  to  label 
them  that  no  complaint  can  be  made  of  misbranding  un- 
der the  food  laws. 

They  are  made  into  the  ordinary  strength  by  a  simple 
reduction  with  alcohol  and  water  in  the  following  pro- 
portions : 

Concentrated  pineapple  ether 3  ounces 

Spirits    J/£  gallon 

Water     J^  gallon 

Dissolve  the  ether  in  the  alcohol,  and  gradually  add  the 
water  and  filter. 


52  Laboratory  Notes 


Laboratory  Notes 

Menstruums  (Solvents). 

Alcohol,  being  the  most  extensively  employed,  will  be 
considered  first.  Alcohol  is  a  volatile,  inflammable,  color- 
less liquid  (C2H5OH)  of  a  penetrating  odor  and  burning 
taste.  In  commerce  the  alcohol  produced  from  maize  or 
other  grain  is  known  as  ethyl  or  grain  alcohol.  It  should 
be  kept  in  well  stoppered  containers,  and  in  a  cool  place, 
remote  from  fire.  When  alcohol  and  water  are  mixed  to- 
gether, a  rise  in  temperature  and  contraction  in  volume 
take  place.  In  small  operations  the  contraction  is  gen- 
erally disregarded;  in  larger  operations  the  loss  is  very 
apparent.  If  fifty-five  gallons  of  alcohol  be  mixed  with 
forty-five  gallons  of  water,  the  total  will  not  be  100  gal- 
lons of  dilute  alcohol,  but  only  96%  gallons,  showing  a 
loss  of  3^4  gallons. 

One  gallon  of  190  proof  alcohol,  temperature  15.6°  C. 
(60°  F.),  specific  gravity  0.816,  weighs  6  pounds  12 
ounces  and  339  grains. 

Proof  Spirit  is  a  term  used  by  the  Revenue  Depart- 
ment in  assessing  the  tax  on  alcoholic  liquors.  It  means 
a  liquid  in  which  there  is  50  per  cent,  (by  volume)  of 
absolute  alcohol.  As  it  is  the  actual  alcohol  in  the 
whiskey,  brandy,  dilute  alcohol,  etc.,  which  is  taxed,  and 
as  this  varies  widely,  it  is  necessary  that  the  actual  wine 
gallons  be  converted  into  proof  gallons  before  the  tax 
rate  can  be  fixed.  A  sample  that  is  half  alcohol  and  half 
water  is  "100  proof."  A  sample  that  is  three-quarters 
alcohol  and  one-quarter  water  is  150  proof,  and  the  tax 
on  every  gallon  of  it  is  one  and  a  half  times  the  regular 
Government  rate  per  proof  gallon.  Absolute  alcohol  is 


Alcohol  S3 

200  proof  and  is  required  to  pay  a  double  tax.  The  legal 
definition  of  proof  spirit  is :  "That  alcoholic  liquor 
which  contains  one-half  its  volume  of  alcohol  of  a  specific 
gravity  of  0.7939  at  60°  F." 

Rule  for  Diluting  Alcohol  (Pile's). 

To  reduce  alcohol  to  any  desired  strength:  To  as 
many  parts  of  the  given  alcohol  as  are  indicated  by  the 
percentage  required,  add  sufficient  water  to  make  the 
number  of  parts  of  the  mixture  equal  to  the  percentage 
of  the  given  alcohol. 

Example:  If  it  is  desired  to  make  an  alcohol  of  30 
per  cent,  from  one  of  95  per  cent.,  take  30  fluid  ounces 
of  the  alcohol  and  add  a  sufficient  amount  of  water  to 
make  95  fluid  ounces. 

The  alcohol  best  suited  for  the  manufacture  of  flavor- 
ing extracts  is  what  is  known  as  true  deodorized  or  Co- 
logne spirit,  or  alcohol  free  from  fusel  oil.  A  mixture 
of  10  cubic  centimeters  of  alcohol  and  0.2  cubic  centi- 
meter of  potash  lye  evaporated  down  to  one  cubic  centi- 
meter should  not  give  any  odor  of  fusel  oil  after  super- 
saturation  with  dilute  sulphuric  acid.  Deodorized  alco- 
hol should  not  possess  a  foreign  odor  and  should  mix 
with  water  without  becoming  turbid. 

Water  as  a  solvent  in  flavoring  extracts  is  next  in 
importance.  Ordinary  water  always  contains  solid  mat- 
ter, and  traces  of  various  salts  in  solution  or  suspension ; 
while  this  solid  matter  and  salts  do  not  ordinarily  unfit 
it  for  drinking  purposes,  they  do,  in  many  instances, 
seriously  interfere  with  the  preparation  of  flavoring  ex- 
tracts. In  some  sections  of  the  country,  the  drinking 
water  might  be  pure  enough  for  the  processes,  or,  at 
least,  it  does  not  contain  serious  impurities ;  in  other  sec- 
tions, the  water  would  be  totally  unfit  for  the  preparation 


54  Laboratory  Notes 

of  flavoring  extracts.    Soft  or  distilled  waters  are  always 
to  be  perferred. 

Brief  Rules  for  Qualitative  Tests  of  Water. 

No.  i.  If  the  water  reddens  blue  litmus  paper  be- 
for  boiling  but  not  afterward,  and  the  color  of  reddened 
paper  is  restored  upon  warming,  it  is  carbonated. 

No.  2.  If  it  possesses  a  nauseous  odor  and  gives  a 
black  precipitate  with  acetate  of  lead,  it  is  sulphurous. 

No.  3.  If  it  restores  blue  color  to  litmus  paper  after 
boiling,  or  develops  a  red  color  on  the  addition  of  a 
phenolphthalein  test  solution,  it  is  alkaline. 

No.  4.  If  it  possesses  neither  of  the  above  proper- 
ties in  a  marked  degree  and  leaves  a  large  residue  upon 
evaporation,  it  is  a  saline  water. 

When  water  is  pure,  it  will  not  become  turbid  or  pro- 
duce a  precipitate  with  any  of  the  following  reagents : 

Baryta  water,  if  a  precipitate  or  opaqueness  appears, 
carbonic  acid  is  present. 

Chloride  of  barium  indicates  sulphates. 

Nitrate  of  silver  indicates  chlorides. 

Oxalate  of  ammonia  indicates  lime  salts. 

Boiling  for  five  minutes  and  filtering  when  cool  will, 
in  many  instances,  make  objectionable  water  suitable  for 
extract  purposes. 

FILTRATION. 

Filtration  is  the  process  of  separating  liquids  from 
solids,  with  the  object  of  obtaining  a  liquid  in  a  trans- 
parent condition.  The  intervention  of  porous  substances, 
termed  filters,  to  intercept  solid  particles  is  necessary  in 
performing  this  process.  They  are  usually  made  from 
paper,  paper  pulp,  linen,  felt,  etc.  Paper  filters  are  the 


Filtration  Methods  55 

most  useful  of  all  kinds  and  are  employed  in  general 
operations  requiring  fine  filtration,  since  the  solid  par- 
ticles are  much  more  completely  separated  by  paper  than 
by  strainers,  owing  to  the  pores  of  the  paper  being 
smaller  and  more  numerous. 

When  folding  a  filter,  care  should  be  observed  not  to 
extend  the  creases  entirely  to  the  apex,  but  to  terminate 
them  at  a  distance  of  about  J^  inch  from  it,  since  the 
point  at  which  all  creases  converge  would  thereby  be  so 
weakened  that  the  weight  of  the  liquid  would  rupture  the 
filter.  When  pouring  the  liquid  in  the  filter,  the  stream 
should  never  be  delivered  upon  the  apex,  but  upon  the 
sides,  feeding  in  a  circular  motion,  so  that  the  force  of 
the  fall  will  be  broken  before  the  weakest  point  is  reached. 
In  filtering  liquids  composed  mostly  of  water  the  paper 
is  very  liable  to  be  broken,  since  the  water  tends  to  soften 
it  (while  alcohol  has  a  reverse  action)  ;  the  use  of  a  small 
tuft  of  absorbent  cotton  in  the  apex  of  the  filter  will,  in 
a  large  measure,  overcome  this  trouble.  The  filter  paper 
should  be  entirely  within  the  funnel,  since,  if  the  edge 
of  the  paper  projects  above  the  funnel,  waste  ensues 
from  evaporation  of  volatile  liquids,  as  well  as  from  the 
increased  and  unnecessary  absorption  due  to  the  excess 
of  the  filtering  paper ;  in  addition,  an  untidy  and  careless 
habit  is  formed. 

The  filtering  papers  in  the  market  are  of  three 
weights :  light,  medium  and  heavy ;  and  of  two  colors : 
white  and  gray.  For  general  purposes  the  French  filters 
are  almost  universally  used,  the  "Prat  Dumas"  brand  be- 
ing the  most  common.  The  gray  filters  are  made  from 
a  mixture  of  cotton,  flax,  wool,  etc.,  and  are  well  adapted 
for  filtering  colored  liquids  or  tinctures,  but,  owing  to 
the  coloring  matter  they  contain,  they  are  not  practicable 
for  liquids  containing  free  alkali.  Ribbed-glass  funnels 


56  Laboratory  Notes 


are  always  to  be  preferred,  as  they  operate  more  rapidly 
than  the  plain.  Felt  filters  are  made  bag-shaped  and  are 
admirably  adapted  in  operations  where  a  large  amount 
of  liquid  is  to  be  filtered  and  in  cases  where  a  filtering 
medium  is  employed.  They  are  made  in  sizes  ranging 
from  one  to  five  gallons'  capacity,  and  operate  very 
rapidly.  When  using  such  a  filter  on  volatile  liquids  it 
should  be  enclosed  in  a  tight-fitting  filtering  cabinet,  pro- 
vided with  a  glass  door ;  for,  if  this  is  not  done,  the  evapo- 
rative loss  due  to  the  large  surface  exposed  to  the  atmos- 
phere will  be  quite  large.  Filtering  mediums  are  finely 
powdered  substances  used  to  facilitate  the  operation  of 
filtering.  They  operate  on  the  principle  of  adhering  to 
or  entangling  the  objectionable  suspended  matter,  thereby 
preventing  it  from  rapidly  obstructing  the  pores  of  the 
filter. 

The  following  substances  are  generally  used  for  this 
purpose :  Magnesium  carbonate,  purified  talcum,  washed 
pumice,  precipitated  calcium  carbonate,  precipitated  cal- 
cium phosphate  and  kieselguhr  (an  infusorial  earth). 
For  operations  on  liquids  containing  acids,  talcum  and 
pumice  are  recommended,  since  the  employment  of  the 
carbonates  results  in  a  chemical  change. 

Filtering  liquids  of  a  volatile  character  should  be  con- 
ducted in  the  least  possible  time,  and,  to  facilitate  this 
condition,  the  filter  must  constantly  be  kept  full,  so  that 
the  maximum  benefit  of  the  filter  surface  can  be  utilized. 
For  this  purpose  the  automatic  feeding  or  continuous  fil- 
tration principle  is  recommended  (see  figure).  The  use 
of  the  containers  termed  skeleton  demijohns  is  especially 
recommended.  The  bottles  are  clear  glass,  affording  op- 
portunity for  minute  and  intelligent  inspection  of  the 
contents.  The  protection  against  breakage  at  the  bottom 
is  perfect,  while  the  four  upright  canes  or  standards  af- 


Filtration  Methods 


57 


ford  security  for  the  sides  and  serve  as  substantial  han- 
dles. These  bottles  are  made  in  three  sizes :  two,  three, 
and  five  gallons'  capacity,  respectively. 

The  capacity  of  the  container  does  not  affect  the  prin- 
ciple involved,  but  in  all  cases  both  bottles  should  be  of 
the  same  capacity,  since,  under  such  conditions,  the  oper- 
ations can  be  conducted  over  night  and  on  Sunday,  with- 
out the  danger  of  overflowing  the  receiver.  This  process 
is  adapted  equally  for  use  with  the  felt  or  other  forms  of 
filters.  In  principle,  when  the  apparatus  is  in  action,  the 
liquid  cannot  escape  from  the  upper  container  after  the 
funnel  is  full  as  high  as  the  mouth  of  that  container,  for 
the  simple  reason  that  the  liquid  in  the  funnel  regulates 
the  ingress  of  air.  After  the  liquid  escapes  through  the 
filter,  receding  from  the  mouth  of  the  inverted  container, 
air  rushes  in,  more  liquid  runs  out,  and  the  supply  in  the 
funnel  is  thus  kept  up  automatically  until  all  the  liquid 
has  run  from  the  upper  bottle  or  demijohn. 


Laboratory  Notes 


PRESSURE  FII/TER  AND  PERCOLATOR 


Double  Pressure  Filter  and  Percolator  59 


DOUBLE  PRESSURE  FILTER  AND  PER- 
COLATOR. 

(See  Fig.,  page  58.) 

In  all  filtering  operations  of  15  gallons  or  more,  the 
most  satisfactory  results  are  obtained  with  the  use  of 
the  Double  Pressure  Filter  and  Percolator,  operating  on 
the  following  principle :  Cocks  "E"  and  "G"  are  closed 
while  vent  valve  "C"  is  opened ;  the  material  to  be  filtered 
or  percolated  is  next  placed  on  perforated  disc  (clothed 
with  felt  or  paper)  "A,"  drawing  off  samples  at  cock  "G" 
and  returning  until  the  filtrate  or  percolate  runs  perfectly 
clear.  At  this  stage,  close  cock  "G"  and  when  the  liquid 
in  space  "B"  reaches  about  10  inches  in  height,  close 
valve  "C"  and  open  cock  "E."  A  portion  of  the  liquid 
will  rapidly  flow  into  receiver  "H,"  but  in  the  absence  of 
sufficient  vent,  a  partial  vacuum  is  formed  in  space  "B" 
and  henceforth  the  flow  into  the  receiver  is  in  ratio  to  the 
flow  through  the  perforated  disc  "A."  Thus  we  have  a 
double  pressure,  viz. :  the  weight  of  the  liquid  on  top  of 
the  disc,  plus  the  partial  vacuum,  or,  as  it  is  ordinarily 
understood,  the  suction  of  the  lower  column  of  liquid, 
the  operation  thus  producing  a  finer  filtrate  in  a  shorter 
period.  The  cock  "G"  is  designed  for  use  in  determining 
the  character  of  the  filtrate  at  the  beginning  of  the  opera- 
tion, as  before  stated;  also  as  an  exit  for  waste  water 
when  washing  out  the  apparatus.  The  glass  gauge  "D," 
while  not  a  necessity,  will  be  found  a  convenience.  All 
fittings  should  be  of  brass,  preferably  tinned. 

To  construct  a  filter  of  this  type,  proceed  as  follows : 
Select  an  alcohol  barrel  in  good  condition;  carefully  re- 
move the  head;  next  thoroughly  remove  all  of  the  glue, 
if  any.  Next  bore  a  ^2-inch  hole  in  the  bottom  and  se- 


6o  Laboratory  Notes 


curely  fasten  a  J^-inch  flange  coupling  and  insert  a  brass 
nipple  so  that  the  end  will  come  up  flush  on  the  inside, 
providing  means  for  thoroughly  draining;  on  this  nipple 
fasten  the  cock.  Insert  a  nipple  at  "E"  and  use  lock 
nuts  on  both  sides  to  thoroughly  secure  it,  and  screw 
on  the  cock.  In  a  like  manner,  insert  a  nipple  for  vent 
pipe  "C,"  bring  up  to  top  of  barrel  and  end  with  valve. 

Should  you  decide  to  use  a  glass  gauge,  it  will  be 
necessary  to  place  it  at  this  time.  The  wood  disc  should 
be  made  of  ^-inch  oak  and  securely  fastened  at  the  cen- 
ter of  the  barrel;  it  should  be  made  in  two  sections  to 
facilitate  placing  it  in  position.  This  disc  should  contain 
a  very  liberal  amount  of  perforations  of  about  %-inch 
diameter;  the  more  perforations  the  better.  After  this 
is  completed,  the  entire  disc  should  be  clothed  with  a 
piece  of  thick  felt  or  paper,  securely  fastened  around  the 
entire  circle ;  the  filter  is  then  ready  for  use.  A  filter  of 
this  design  can  be  constructed  of  metal,  but  oak  is  much 
preferable  on  extract  work,  particularly  vanilla. 

When  through  with  the  filter,  always  clean  it  at  once 
in  the  following  manner:  Remove  all  of  the  magma 
(solids)  from  the  filtering  disc,  next  add  hot  water  and 
operate  as  in  filtering,  with  the  exception  of  drawing  off 
at  cock  "G,"  and,  when  through,  leave  all  portions  of 
the  filter  open  to  the  air,  including  valves  and  cocks, 
thereby  eliminating  the  tendency  of  the  formation  of 
must  and  foreign  odors.  A  filter  of  this  class  will  operate 
with  the  minimum  evaporative  loss,  since  the  liquids  at 
no  time  are  exposed  to  the  atmosphere,  and  can  be  fed 
automatically  from  an  exterior  source  (an  inverted  con- 
tainer or  syphon).  The  labor  for  results  obtained  is  the 
minimum  and  the  filter  will  last  for  years.  The  receiver 
should,  in  all  cases,  be  of  the  same  capacity  as  the  amount 
operated  on,  thus  eliminating  any  danger  of  overflowing. 


Simple  Methods  of  Testing  61 


SIMPLE  METHODS  OF  TESTING. 

The  presence  of  fixed  (fatty)  oils,  such  as  poppy- 
seed,  castor  and  other  bland  resinous  oils,  can  readily  be 
determined  by  placing  a  few  drops  on  clean  white  blot- 
ting paper  and  exposing  the  paper  to  a  mild  heat ;  if  the 
oil  is  pure,  the  spot  on  the  blotter  disappears  immediately. 
To  fully  substantiate  this  test  the  blotter  should  be  held 
up  to  the  light,  and  if  no  permanent  stain  is  visible,  the 
oil  can  be  accepted  as  free  from  fixed  oils. 

Alcohol  is  sometimes  added  to  essential  oils  of  high 
value.  To  detect,  add  a  small  portion  in  a  graduated  test 
tube  and  carefully  drop  in  a  small  amount  of  water;  if 
alcohol  is  present,  the  drops  will  be  surrounded  with  a 
milky  (turbid)  circle;  next,  add  more  water  and  shake, 
and  after  the  liquids  have  separated,  the  approximate  per 
cent,  of  alcohol  present  can  be  computed  by  the  increased 
volume  of  the  upper  layer.  Another  method  consists  of 
agitating  with  the  oil  in  a  test  tube  a  few  small  pieces  of 
dried  chloride  of  calcium.  These  will  remain  unchanged 
if  the  oil  is  pure,  but  they  will  dissolve  in  an  oil  contain- 
ing alcohol,  and  the  resulting  solution  will  form  a  dis- 
tinctive layer  on  the  bottom  of  the  container. 

A  more  accurate  test  of  the  presence  of  alcohol  in  an 
essential  oil  is  accomplished  by  the  use  of  metallic  sodium 
or  potassium.  Place  fourteen  drops  of  the  oil  on  a  per- 
fectly dry  watch  glass,  and  put  a  piece  of  sodium  or  po- 
tassium, the  size  of  a  pin's  head,  in  the  center  of  it.  If 
the  alkali  remains  unchanged  for  twenty  minutes,  no  al- 
cohol is  present,  but  if  it  disappears  after  five  minutes, 
the  oil  contains  at  least  4  per  cent,  of  alcohol;  if  it  dis- 
appears in  less  than  one  minute,  it  indicates  the  presence 
of  not  less  than  20  per  cent,  of  alcohol. 


62  Laboratory  Notes 


To  Test  Oil  of  Lemon. — The  presence  of  purified 
turpentine  in  oil  of  lemon  is  not  so  easily  detected  on 
account  of  its  similar  composition  and  specific  gravity. 
By  adding  three  volumes  of  strong  alcohol  with  one  vol- 
ume of  the  oil,  the  turpentine,  if  present,  will  remain  un- 
dissolved,  and  by  evaporating  a  small  quantity  on  a  blot- 
ting paper  and  shaking  the  paper  in  the  air,  the  presence 
of  this  adulterant-  will  be  indicated  by  the  terebinthinate 
(turpentine)  odor,  using  a  similar  test  for  comparison 
with  an  oil  of  known  purity. 

The  most  dangerous  adulterant  in  oil  of  lemon  is 
citrene,  the  terpene  principle  obtained  as  a  by-product  in 
the  extraction  of  citral  from  oil  of  lemon,  while  prepar- 
ing terpeneless  oil. 

To  Test  the  Purity  of  Oil  of  Cloves. — Oil  of  cloves, 
when  pure,  will  manifest  the  following  reaction :  When 
shaken  with  pure  liquor  of  ammonia,  it  coagulates  and 
crystallizes  after  fusion  by  a  gentle  heat ;  treated  with  an 
alcoholic  solution  of  potassa,  it  congeals  into  a  crystalline 
mass  with  total  loss  of  its  odor.  A  solution  of  potassium 
chromate  transforms  it  into  brown  flakes,  while  the  yel- 
low color  of  the  salt  is  dissipated.  A  negative  result  in- 
dicates an  addition  of  inferior  oils. 

To  Test  the  Purity  of  Oil  of  Bitter  Almonds. — Oil  of 
bitter  almonds  is  sometimes  adulterated  with  nitro-ben- 
zole,  and  this  may  be  detected  by  the  use  of  a  solution  of 
potassa.  The  liquid  has  a  green  color  if  nitrate-benzole 
is  present,  and  upon  dilution  three  layers  are  formed,  the 
lower  yellow,  the  upper  green ;  over  night,  the  green  color 
changes  to  red. 

To  Test  the  Purity  of  Otto  of  Roses. — The  principal 
adulterants  to  be  found  in  otto  of  roses  are  the  oils  of 
rhodium,  geranium,  sandalwood  and  camphor,  and  occa- 
sionally spermaceti,  which  is  added  to  contribute  the  crys- 


Simple  Methods  of  Testing  63 


talline  appearance.  Otto  of  rose,  when  pure,  has  a  bland, 
sweet  taste;  if  it  is  bitter,  this  indicates  the  presence  of 
rhodium  or  sandalwood ;  if  it  is  pungent  or  biting  to  the 
palate,  it  contains  either  oil  of  geranium  or  camphor,  or 
both ;  if  it  imparts  an  unctuous  sensation  to  the  palate,  or 
if  it  responds  to  the  blotter  paper  test  for  fixed  oils,  it 
contains  spermaceti.  A  single  drop  of  otto,  placed  on  a 
watch  glass  with  one  drop  of  concentrated  sulphuric  acid 
(C.  P.)  and  stirred  with  a  glass  rod,  will  retain  its  purity 
and  color,  but  a  sample  adulterated  with  other  oils  is  ren- 
dered more  or  less  brown  and  develops  peculiar  odors, 
i.  e.,  from  oil  of  geranium,  strong  and  disagreeable ;  from 
oil  of  rhodium,  increased  and  rendered  unctuous  and  re- 
sembling cubeb;  from  camphor,  characteristic  and  com- 
bined with  acidity ;  from  spermaceti,  unctuous  and  clearly 
perceptible. 

The  specific  gravity  of  an  essential  oil  is  not  an  in- 
fallible indicator,  and  this  method  should  be  employed 
only  after  all  other  known  methods  of  detection  have 
been  resorted  to. 


64  Laboratory  Notes 


ESTIMATION    OF    SMALL    QUANTITIES    OF 
ESSENTIAL  OILS. 

To  determine  the  per  cent,  of  essential  oil  in  flavor- 
ing extracts,  proceed  as  follows : 

Howard  Method. — Twenty  c.c.  of  the  extract  are 
diluted  with  50  c.c.  of  water  and  one  drop  of  hydrochloric 
acid  (except  in  case  of  clove  and  cinnamon  extracts, 
when  the  acid  is  unnecessary).  The  liquid  is  then  ex- 
tracted in  a  separator  with  three  successive  portions  of 
15  c.c.,  10  c.c.  and  5  c.c.  of  ether.  The  mixed  ethereal 
extracts  are  washed  with  10  c.c.  of  water  that  has  been 
previously  saturated  with  ether,  so  as  to  remove  prac- 
tically all  of  the  alcohol.  The  ether  solution  is  now  trans- 
ferred to  a  Babcock  milk  bottle,  which  is  immersed  in 
warm  water  and  the  ether  driven  off.  Water  is  now 
added  and  the  bottle  is  placed  in  the  centrifugal  ap- 
paratus, and  the  essential  oil  read  off  in  the  bottle  in  the 
same  way  as  with  milk  fat.  The  author  claims  that  this 
process  renders  very  accurate  results,  as  the  essential  oil 
is  scarcely  exposed  to  heat,  and  there  is,  therefore,  little 
risk  of  loss  by  evaporation. 

TO  DETERMINE  THE  PER  CENT.  OF  GAS  IN 
AQUA-AMMONIA. 

The  "Baume"  hydrometer  for  ammonia  renders  fairly 
good  results,  provided  no  alkaline  salts  to  any  appreciable 
extent  are  present;  this  condition  cj,n  be  determined  by 
evaporation  over  a  steam  bath.  For  comparative  testing 
the  use  of  the  burette  will  be  found  more  accurate,  using 
a  standard  acid  solution  in  the  burette  and  15  c.c.  of  am- 
monia with  a  drop  of  phenolphthalein  indicator  added  to 
it,  and  continuing  the  flow  until  exactly  neutralized. 


Determining  Acidity  of  Vinegar  65 


TO  DETERMINE  THE  PER  CENT.  OF  ACIDITY 
(AS  ACETIC  ACID)  OF  VINEGAR. 

Fill  a  50  c.c.  burette  to  zero  point  with  "standard  al- 
kali solution."  Fill  pipette  by  suction  with  vinegar  to  be 
tested ;  cover  mouth  end  with  finger  and  allow  the  vinegar 
to  fall  exactly  to  6  c.c.  mark  and  place  the  vinegar  in  a 
porcelain  dish  until  exactly  at  zero  mark.  Add  a  little 
pure  water  to  the  vinegar  (distilled  preferable)  until 
nearly  colorless;  next  add  a  drop  of  indicator,  and  by 
opening  the  pinch-cock  add  standard  alkali  solution  from 
the  burette  until  a  permanent  faint  pink  color  appears, 
stirring  with  glass  rod  meanwhile.  With  a  45-grain 
(4.5%)  vinegar,  about  40  c.c.  of  alkali  solution  may  be 
quickly  added  to  the  vinegar;  then  it  should  be  added, 
drop  by  drop,  until  a  faint  pink  color  is  permanent.  The 
number  of  c.c.  of  alkali  solution  used  indicates  the  acid 
strength  in  grains,  which,  divided  by  ten,  gives  per  cent, 
of  acidity  (as  acetic  acid).  For  a  strong  vinegar  (over 
50  grains)  fill  the  pipette  to  3  c.c.  mark  only  and  multiply 
the  burette  reading  by  two. 

The  "standard  alkali  solution"  used  for  the  above 
test  can  be  obtained  from  any  reliable  consulting  chemist 
or  dealer  in  chemical  supplies,  and  is  known  as  a  tenth- 
normal  alkali  solution,  being  a  0.4  per  cent,  solution  of 
sodium  hydrate,  very  exactly  standardized,  against  tenth- 
normal  acid  which  has,  in  turn,  been  exactly  standardized 
by  calcite  or  other  scientific  means. 

The  indicator  solution  is  prepared  by  dissolving  about 
2  per  cent,  of  the  phenolphthalein  in  strongest  alcohol 
and  diluting  with  an  equal  volume  of  distilled  water. 


66  Laboratory  Notes 


TO  PURIFY  ESSENTIAL  OILS  DETERI- 
ORATED FROM  AGE. 

There  are  several  oils  that  by  absorption  of  oxygen 
from  the  air  and  from  the  chemical  effect  of  light  rays 
will  become  camphorated,  grow  turbid,  deposit  a  residue 
(generally  called  stearopten)  and  lose  more  or  less  of 
their  natural  flavor,  and,  in  the  case  of  lemon  oil,  will 
acquire  the  odor  of  crude  turpentine.  Such  oils  as  are 
free  from  oxygen  are  chiefly  subject  to  these  changes. 
Oils  that  have  deteriorated  in  the  manner  indicated  may 
be  improved,  but  they  can  never  be  fully  restored  to 
their  original  condition. 

There  are  various  methods  employed:  The  most 
practicable  is  redistillation,  mixing  the  oils  first  with 
water  and  incorporating  a  small  amount  of  alkali ;  or  by 
agitation  for  thirty  minutes  with  a  thick  paste  consisting 
of  powdered  borax,  animal  charcoal  and  water,  and  fil- 
tering. The  latter  process  renders  excellent  results  with 
almost  all  essential  oil  restorations.  Another  method  is 
to  add  10  per  cent,  of  warm  water,  shake  well  for  fifteen 
minutes,  let  settle,  draw  off  by  means  of  a  syphon,  and 
filter  through  paper.  Another  process  is  the  use  of  a 
potassium  permanganate  solution  as  follows:  Dissolve 
one  ounce  of  the  salt  in  seven  ounces  of  water  and 
thoroughly  agitate  with  four  pounds  of  the  oil,  decant, 
mix  with  fresh  water,  and  heat  gently  until  the  oil  as- 
sumes a  clear  condition ;  then  separate  and  filter. 


Miscellaneous  Receipts  67 

MISCELLANEOUS  RECEIPTS. 

PLAIN  OR  SIMPLE  SYRUP. 

Granulated  cane  sugar 30  pounds 

Water  (boiling)    7  quarts 

Pour  the  sugar  into  the  water  gradually,  stirring  mean- 
while, and  when  dissolved,  strain  through  coarse  cotton 
cloth.  Do  not  cover  container  until  thoroughly  cooled. 
This  will  produce  four  gallons  of  syrup.  The  relative 
proportions  of  sugar  and  water  are  very  important  since, 
if  a  smaller  amount  of  sugar  is  employed,  fermentation 
sooner  or  later  will  ensue.  If  too  much  sugar  is  used, 
crystallization  will  surely  follow,  resulting  in  a  liquid  too 
thin  to  keep  under  ordinary  temperature. 

SODA  FOAM. 

Soap  bark,  chips  or  coarse  ground .   1 24  pounds 

Alcohol,  190  proof 2      pints 

Water,  quantity  sufficient  to  make.    I       gallon 

Mix  the  bark  with  6  pints  of  water,  boil  for  10  minutes 
and  strain.  Add  enough  water  (hot)  through  the  strainer 
to  make  6  pints  of  tincture  and  when  cool  add  the  alco- 
hol. Let  stand  over  night  and  filter.  One  fluid  ounce  of 
this  tincture  is  sufficient  for  one  gallon  of  syrup. 

FRUIT    ACID    SOLUTION. 

Citric  acid  in  crystals 2  pounds 

Alcohol,  190  proof I  pint 

Water  (distilled  preferred)  to  make.    I  gallon 

Dissolve  the  acid  in  the  water,  add  the  alcohol,  set  aside 
for  a  few  hours,  and  filter  through  paper.  One  ounce  of 
this  is  sufficient  for  one  gallon  of  syrup. 


68  Laboratory  Notes 

For  soda-fountain  syrups,  add  from  2  to  4  ounces  of 
flavor  and  color  to  suit. 

SEALING  OR  BOTTLE-TOPPING   WAX. 

No.  i. — Elastic  Enamel  Wax. 

Good  white  glue i       pound 

Oxide  of  zinc i       ounce 

Precipitated  chalk   i       ounce 

Dry  white  lead J/2  ounce 

Glycerine  3      ounces 

Color  to  suit. 

Make  a  paste  of  zinc,  chalk  and  glycerine  by  rubbing 
them  up  into  a  cream ;  then  stir  them  into  the  liquid  glue 
while  hot  and  to  about  the  consistency  of  syrup,  and  stir 
thoroughly ;  it  is  then  ready  for  use  in  the  white  and  can 
be  colored  any  shade  desired  by  using  aniline  to  suit. 
Antique  bronze  color  can  be  obtained  first  by  adding  a 
little  dry  bronze  powder  and  then  adding  aniline  of  the 
shade  desired.  To  be  used  warm  over  water  bath,  and 
can  be  used  any  number  of  times. 

No.  2. 

Rosin 40  pounds 

Silicate  of  magnesia 25  pounds 

Paraffine   2  pounds 

Color  to  suit. 

Dissolve  the  rosin  and  paraffine  with  the  aid  of  heat ;  stir 
in  the  silicate  of  magnesia,  stirring  until  thoroughly  in- 
corporated; next  add  the  color. 

No.   3.     Take   ordinary   hard   paraffine   and,   when 
melted,  stir  in  sufficient  oil  soluble  and  aniline  to  suit. 

GRADUATING  CONTAINERS. 

Graduated  containers  will  be  found  very  convenient 


Miscellaneous  Receipts  69 

when  used  as  receivers  in  filtration  or  percolation  opera- 
tions, or  for  use  in  compounding.  Plain  containers  may 
be  graduated  by  placing  them  in  a  perfectly  level  position 
and  carefully  measuring  out  the  exact  quantity  of  water 
at  60  degrees  F.,  next  pasting  a  strip  of  bright-red-colored 
paper  on  the  four  quarter  points,  being  careful  to  allow 
for  the  capillary  curves ;  and,  when  dry,  shellacking  the 
surface  of  the  paper. 

DEODORIZING  CONTAINERS. 

Place  in  the  container  some  mashed  raw  potatoes  with 
warm  water,  and  shake  occasionally  for  one  hour;  then 
empty  the  contents  and  wash  with  cold  water.  The  odor 
will  then  have  entirely  disappeared.  Such  obstinate  odors 
as  peppermint  readily  yield  to  this  treatment.  To  clean 
containers  from  the  dry,  hard  film  frequently  encoun- 
tered, use  a  solution  of  potash  with  fine  shot.  This  is  also 
useful  in  removing  fixed  oils,  etc. 


70  Laboratory  Notes 


ADHESIVES. 

As  a  matter  of  convenience  it  is  always  desirable  to 
employ  an  adhesive  that  can  be  used  in  the  cold  and,  at 
the  same  time,  that  will  dry  in  the  shortest  possible  time. 
The  best  article  for  use  on  carton  work  is  "silicate  of 
soda";  it  is  inexpensive,  does  not  ferment  or  decompose 
and  will  render  very  satisfactory  results.  Another  good 
preparation  is  powdered  corn  starch  digested  with  the 
aid  of  an  alkali ;  however,  considerable  care  is  necessary 
in  its  preparation,  since  it  is  highly  important  that  the 
minimum  possible  amount  of  alkali  should  be  employed 
as  per  the  following : 

Into  a  suitable  receptacle  place  one-half  gallon  of  cold 
water;  next  stir  in  one  pound  of  powdered  corn  starch 
and  follow  with  one-half  gallon  of  boiling-hot  water  into 
which  has  been  added  three  fluid  ounces  of  alkali  solu- 
tion; stir  until  the  mass  becomes  clear  and  transparent 
and  immediately  reduce  to  the  consistency  desired  with 
hot  water.  For  carton  work  it  should  be  used  consider- 
ably heavier  than  for  labeling.  This  paste  will  not  fer- 
ment or  decompose,  and  is  very  economical,  but,  as  be- 
fore stated,  requires  considerable  care  in  its  preparation. 

ALKALI  SOLUTION    (FOR  PASTE). 

Dissolve  Red  Seal i  can 

Lye  in  water i  quart 


Weights  and  Tables 


TABLES. 

AVOIRDUPOIS  WEIGHT. 
Pounds.          Ounces.  Drachms.       Grains  (Troy). 

i     =      16     =     256     =     7,000 
i     =       16     =        437.5 
i     =          27.34 


Grams. 
453-60 

28.35 
1.77 


FLUID   MEASURE. 
Gallons.     Pints.       Ounces.  Drams.  Minims. 

i    =  8  =    128  =    1,024 
i   =     16  =      128 


Cubic  Centimeters. 
=    6l,440    =     3,785.435 
473-179 


=   7,680  = 


480 
60 


29-574 
3.697 


Sixteen  ounces,  or  one  pint,  is  sometimes  termed  a 
fluid  pound.    The  above  table  is  the  one  usually  adopted 


in  formulas. 

Pounds  of  Sugar. 
Added  to 
One  Gci  lion  of 

Quantity 

SYRUP  TABLE. 

of    Syrup   Actually 

Obtained. 

Pounds  of 
Sugar  in 

Cold  Water. 

Gallons. 

Pints.           Fluid  Ounces. 

of  Syrup. 

I 

I 

10 

•93 

2 

I 

I 

4 

i-73 

3 

I 

I 

14 

2-43 

4 

I 

2 

3 

3-05 

5 

I 

3 

2 

3-6 

6 

I 

3 

12 

4.09 

7 

I 

4 

6 

4-52 

8 

I 

5 

.  . 

4.92 

9 

I 

5 

10 

5-28 

10 

I 

6 

4 

5-62 

ii 

I 

6 

14 

5-92 

12 

I 

7 

8 

6.18 

13 

2 

2 

6.38 

14 

2 

12 

6.7 

15 

2 

i 

6 

6.91 

72  Laboratory  Notes 


AQUA  (HOUSEHOLD)  AMMONIA. 

Ammonia  is  a  colorless,  pungent,  suffocating  gas 
(NH3),  and  the  commercial  article  is  obtained  from  gas 
liquor.  Water  is  capable  of  absorbing  670  times  its  vol- 
ume of  ammonia  gas  at  50  degrees  F.,  increasing  in  bulk 
about  two-thirds.  Keep  the  tanks  in  a  cool  place  and  the 
plug  secure,  since  heat  rapidly  expands  the  gas,  with 
consequent  loss  and  danger  when  drawing  off.  It  is 
safer,  if  the  ammonia  has  been  kept  in  a  warm  room,  to 
cool  it  off  with  ice  water  before  attempting  to  withdraw 
the  plug,  as  the  liberated  gas,  when  warm,  frequently  is 
forced  out  with  extreme  violence,  and  accidents  which 
have  resulted  in  injury  to  the  sight  of  the  operator  are 
on  record.  The  best  antidote  is  the  exposure  or  inhala- 
tion of  vinegar  or  acetic  acid. 

Table  Showing  the  Percentage  of  Gas  contained  at  60 
Degrees  Fahrenheit. 


20  degrees  Beaume 17     per  cent. 

19        "  "       15        "       " 

18        "  "       13.5     "       " 

17        "  "       12       "       " 

16        "  "       10       "       " 

15        "  "       8       "      " 

14        "  "       6.6    "      " 

j -2        a  «  -       «      « 

12  "  "          3.2      "         " 

ii        "  "       1.6    "      " 

One  gallon  of  26  degrees  weighs  7^2  pounds. 


Bottles  73 


BOTTLES  AND  CORKS. 

BOTTLES— CAPACITY,  BREAKAGE,  ETC. 

The  question  of  over-capacities  and  breakage  of  ex- 
tract bottles  is  of  sufficient  importance  in  that  it  seriously 
affects  the  cost  of  production.  It  is  a  well-known  fact 
that  it  is  next  to  impossible  to  purchase  bottles  accurately 
graduated,  since  the  workman  or  blower  is  compelled  to 
guess  at  the  quantity  of  glass  he  gathers  for  each  bottle. 
He  can  do  nothing  else,  as  it  is  impossible  to  weigh  or 
measure  the  molten  mass.  This  is  why  it  is  impossible  to 
guarantee  the  absolute  accuracy  of  a  bottle.  However, 
some  manufacturers  are  able  to  balance  the  variation  to 
within  about  2  per  cent,  either  way,  and  this  is  about  the 
best  condition  we  can  look  to  until  the  time  when  such  a 
glass-blowing  machine  as  the  "Owens"  will  be  adapted  to 
the  making  of  extract  bottles. 

Breakage  of  bottles  is  due  to  several  causes :  Im- 
proper combination  of  raw  materials,  an  excess  of  silica, 
a  deficiency  of  alkali,  insufficient  heat  in  furnace,  uneven 
distribution,  and  improper  annealing,  since  carelessness 
on  the  part  of  the  lehr  tender  in  not  keeping  his  lehr  at 
the  correct  temperature  will  cause  breakage.  A  large 
amount  of  breakage  is  due  to  rough  handling  in  transit 
by  the  transportation  companies,  draymen  and  receiving 
departments.  The  writer  would  suggest  ordering  bottles 
shipped  in  the  open  crate  with  paper  packing,  in  place 
of  the  closed  box  with  hay  for  packing,  since  in  the  for- 
mer the  men  can  see  what  they  are  handling  and  are  more 
careful  than  they  would  be  with  the  old-style  package. 
The  receiving  department  should  be  very  careful  before 
signing  for  bottle  shipments  to  ascertain  that  the  crates, 
cases  and  contents  are  in  good  condition.  If  not,  they 


74  Bottles 

should  make  a  notation  on  the  receipt  that  the  goods  were 
received  "in  damaged  conditions,  subject  to  claim." 

Bottles  should  always  be  well  washed  prior  to  filling, 
irrespective  of  their  clean  appearance  when  taken  from 
the  packing  case,  for  we  must  not  forget  that  they  are 
intended  to  contain  a  food  product,  and,  since  glass  is  a 
product  resulting  from  a  fusion  at  a  high  temperature  of 
silica  and  alkali,  very  frequently  traces  of  the  alkali  are 
found  in  the  bottles,  and  these  traces  would  have  the  ten- 
dency to  deteriorate  some  of  the  more  delicate  flavors. 

FILLING  BOTTLES. 

Bottle-filling  machines  are  a  valuable  adjunct  to  con- 
cerns handling  a  large  quantity  of  given  size  bottles  at 
one  time.  In  cases  of  frequent  changing  of  containers 
and  material,  a  cheap  method  consists  of  the  use  of  a 
large,  portable  tray  made  of  well-seasoned  wood,  of  suit- 
able length  and  depth  to  accommodate  the  tallest  bottles. 
The  tray  should  be  lined  with  sheet  copper,  although  zinc 
will  answer  the  purpose,  but  will  not  last  as  long.  It 
should  be  fitted  with  standards  of  four  by  four,  and  in- 
clined to  one  of  the  corners,  so  that  any  liquid  spilled  by 
overflow  or  broken  bottle  can  be  quickly  recovered 
through  the  drain.  The  standards  should  be  fitted  with 
roller-bearing  castors  of  at  least  three  inches  diameter. 
This  portable  tray  can  be  run  to  the  bottle  dryer  and 
filled  and  next  run  to  the  source  of  supply  and  the  bot- 
tles filled  and  corked  with  the  aid  of  a  rubber  mallet. 
They  can  then  be  run  to  the  labeling  table  and  either 
labeled  from  the  tray,  or  transferred  to  the  tables,  the 
latter  being  the  better  method,  since  all  bottles  ought  to 
be  permitted  to  lie  flat  on  the  table  for  a  short  time  in 
order  to  ascertain  that  there  are  no  leaky  corks  in  the  lot. 


Filling  Bottles — Corks  75 

When  filling  bottles,  the  supply  should  be  elevated  on 
a  superstructure  at  least  forty  inches  higher  than  the 
portable  tray.  If  the  stock  can  be  contained  in  a  barrel, 
a  suitable-sized  rubber  tube  may  be  connected  with  the 
faucet;  but  in  the  event  of  the  container  being  of  glass, 
the  syphon  system  will  have  to  be  employed,  with  the 
aid  of  a  semi-circular  rubber-tube  supporter  to  obviate 
the  kinking  of  the  tube.  A  certain  percentage  of  the  bot- 
tles will  be  found  to  contain  a  surplus  quantity,  and  these 
can  rapidly  be  corrected  with  the  aid  of  a  wood  displace- 
ment stick.  This  stick  should  be  cut  or  dressed  with  a 
handle  about  J^  inch  diameter  and  iJ/2  inches  long;  at 
this  point  a  shoulder  should  be  provided  and  the  rest 
should  be  of  a  diameter  sufficiently  small  to  enter  the 
bottle  readily  and  of  a  length  to  displace  the  required 
amount;  this  will  necessarily  have  to  be  determined  by 
experiment. 

CORKS. 

Use  a  good  three  or  4  "X"  extra  long  taper  cork. 
Corks  should  be  stored  in  a  dry  room,  as,  in  a  damp  room, 
the  corks  attract  moisture  and,  in  consequence,  molds 
attach  themselves  to  them  and  they  acquire  not  only  an 
unpleasant,  musty  odor,  but  a  bad  taste,  easily  communi- 
cated to  the  contents  of  the  bottles  stoppered  with  them. 
Before  using,  immerse  them  in  cold  water,  never  hot 
water.  Very  frequently  when  removing  a  cork  it  will 
break,  hence  the  advisability  of  placing  in  the  carton  an 
extra  cork. 


76  Figuring  Costs 


FIGURING  COSTS. 

The  common  error  of  computing  costs  of  finished 
products  wholly  on  formulas  and  costs  of  raw  materials 
is  practised  by  quite  a  number  of  concerns.  Shrinkage 
losses,  both  visible  and  otherwise,  are  inevitable  and  must 
be  carefully  considered.  For  example,  when  equal  quan- 
tities of  water  and  alcohol  are  mixed,  a  curious  phenom- 
enon occurs,  since  they  occupy  less  space  than  when  sepa- 
rate, the  shrinkage  amounting  to  about  3 J4  Per  cent. 
This  shrinkage,  being  controlled  entirely  by  nature,  can- 
not, of  course,  be  eliminated.  There  are  other  losses  that 
develop  in  the  manufacture  of  flavoring  extracts,  and 
the  total  content  should  be  determined  in  each  batch  pro- 
duced. This  can  be  readily  ascertained  by  the  use  of  a 
card-recording  system,  as  follows : 


Figuring  Costs  77 


Extract  Department. 
Date,  February  12,  1912. 
Batch  No.  i. 

Character  of  stock  produced,  Tuxedo  brand  vanilla 
Operation  started,  February  12. 
Operation  finished,  February  20. 

Total  gallons  required  from  formula,  22. 
Per  cent,  of  beans  used,  10. 
Character  of  beans  used,  Bourbon,  75  per  cent. 
Character  of  beans  used,  Mexican,  25  per  cent. 
Total  amount  of  beans  used,  17.6  pounds. 
Cost  of  beans  per  pound,  Bourbons,  $3.00. 
Cost  of  beans  per  pound,  Mexicans,  $3.50. 
Per  cent,  of  alcohol  used  in  menstruum,  50. 
Amount  of  finished  product  obtained,  21.25  gallons. 
Amount  of  added  menstruum  required  to  complete, 

.75  gallon. 

Cost  of  same $i  .00 

Total  cost  of  beans 55-O° 

Amount  and  cost  of  alcohol  used,  n  gallons 

@  $2.68   29.48 

Amount  and  cost  of  sugar  used,  20  pounds 

@  .05   i.oo 

Total  labor  required,  5  hours  @  .40 2.00 

Total  cost  for  22  gallons $88.48 

Total  cost  per  gallon 4.03 

Remarks   . 


78  Figuring  Costs 


Extract  Packing  Department. 

Date,  March  5,  1912. 

Character  of  stock  packed,  2  oz.  Tuxedo  vanilla. 

Amount   of    stock    supplied,    14   gallons    @ 

$4-03    • 

Less  23/100  gallons  remaining 93 

Total  cost  of  vanilla $5549 

Bottles  supplied,  6  gross  @  $2.15 12.90 

Bottles  broken,  18 27 

Over-capacity,  2  per  cent. =34.56  ounces. ...  1.02 

Six  gross  of  cartons  @  $3.80  per  1,000 3.28 

Corks  and  labels  i  .60 

Time  required  washing  bottles,  i  girl,  2  40/60 

hours,  @  .  10 27 

Time  required  rilling  bottles,  I  girl,  3  20/60 

hours,®  .11 37 

Time  required  labeling  and  completing,  i  girl, 

12  15/60  hours,  @.ii   1.35 


$76.55 
Total  cost  per  gross 12.76 


To  the  above  should  be  added  a  certain  per  cent,  to 
cover  supervision  and  general  expenses. 


Figuring  Costs  79 


The  essential  advantages  of  the  recording  system  con- 
sist of  providing  ready  means  for  determining  the  yearly 
output,  including  exact  costs,  of  all  grades  of  goods 
manufactured.  It  serves  as  a  check  on  raw  materials, 
including  the  shrinkage  of  alcohol,  vanilla  beans,  etc.,  in 
original  packages,  and  as  an  incentive  to  encourage  em- 
ployees to  provide  means  for  reducing  leaks  and  waste 
to  their  lowest  terms.  It  standardizes  time  requirements 
for  various  operations  and  provides  means  for  deter- 
mining the  relative  values  of  the  employees.  Again,  since 
the  capacities  of  stock  bottles  vary  to  an  appreciable  ex- 
tent, this  system  will  continually  keep  one  in  touch  with 
the  same. 

Count,  Weigh  and  Measure  All  Items  on  Receipt  of 
Shipment. — As  an  illustration:  On  receipt  of  a  barrel 
of  95  per  cent,  alcohol  or  190  proof,  if  the  barrel  has  on 
it  the  Government  stamp,  one  is  reasonably  certain  of 
its  purity.  Weigh  the  barrel  at  once  and  note  if  the 
weight  agrees  with  the  Government  gauger's  weight 
stamped  near  the  bung;  if  it  does  not,  notify  the  distiller 
or  dealer  at  once.  If  the  weight  is  correct,  open  the 
barrel,  and  with  the  aid  of  a  hydrometer  (alcoholometer) 
determine  the  proof.  After  the  barrel  is  empty,  weigh 
it  and  note  if  the  tare  as  stamped  on  the  barrel  is  cor- 
rect, and  if  so,  divide  the  net  pounds  by  6.7963,  represent- 
ing the  weight  of  one  gallon  of  95  per  cent,  alcohol.  The 
author  would  suggest  that  the  alcohol  be  shipped  in  glue- 
coated  barrels,  as  this  prevents  any  solution  from  the 
wood  of  the  barrel,  which,  in  some  instances,  affects  the 
color  and  solvent  properties  of  the  alcohol. 


8o 


Index 


Index 


Acidity  in  Vinegar 65 

Adhesives    76 

African  Vanilla  Beans 14 

Age,  Deteriorated  Essential 

Oils    66 

Ageing  Vanilla   24 

Alcohol..  14,  27,  28,  29,  52, 

53,  61 
Alcoholic  Content  of  Men- 

struums     29,  30 

Allspice   (Pimento)   Ext...  47 

Almond   Extract   8,42 

Almond    Extract,   :|Fede/ral 

Standard    42 

Ammonia   64,  72 

Anise   Extract    8,  47 

Apple   Extract,   Imitation . .     9 

Aqua-Ammonia    64,  72 

Avoirdupois  Weight  71 

Bottle  Breakage    73,74 

Bottle   Capacity    73 

Bottle    Filling    74,  75 

Bottles    73-75 

Bottle   Topping  Wax   For- 
mulas     68,  69 

Bourbon  Vanilla  Beans n 

Brooks  on  Resins 15 

Care  of  Finished  Extracts.  31 

Carton  Adhesives  70 

Cassia  Extract  8,  48 

Celery  Extract  8,  47,  48 

Cherry  Extract,  Imitation.  9 

Chocolate  Extract  49 

Cinnamon  Extract 8,  48 

Circular  No.  19,  U.  S. 

Dept.  of  Agriculture 8 

Classes  of  Extracts 8 

Clove  Extract  49 

Cold  Work  in  Extract 

Making  27 

Coloring,  Use  of 40 

Comoros,  Vanilla  Beans...  15 
Containers,  Deodorizing...  69 
Containers,  Graduating 69 


Corks  75,  76 

Cost   Record,    Extract    De- 
partment      77 

Cost  Record,  Extract  Pack- 
ing Department 78 

Costs    of    Extract    Depart- 
ment   76,  77,  78,  79 

Coumarin   8,  25,  26,  28 

Coumarin   Extract    8,26 

Cultivation  of  Vanilla  Beans   12 
Cutting  Vanilla  Beans 17 

Definition  of  Flavoring  Ex- 
tract         8 

Deodorizing  Containers 69 

Digestion   in   Vanilla   Bean 

Exhaustion   20 

Dilutirig  Alcohol,  Rule  for.  53 
Double  Pressure  Filter  and 
Percolator    59,  60 

Essential  Oil   Extracts ...  8,  48 
Essential    Oils. 8,  32-36,  48,  61, 
62,  63,  64,  66 
Essential  Oils  Deteriorated 

by  Age 66 

Esters    Extracts,    Estimate, 

ing  Small  Quantities  of..     8 
Ethereal,      Imitation      Fla- 
vors    50,  51 

Ethereal  Extracts 8,  9,  50 

Exhaustion  of   the  Vanilla 

Bean  4 17 

Extract    of    Allspice     (Pi- 
mento)      47 

Extract  of  Almond    8,  42 

Extract  of  Anise   47 

Extract  of  Cassia    48 

Extract  of  Celery  47,  48 

Extract  of  Chocolate    49 

Extract  of  Cinnamon   48 

Extract  of  Cloves    49 

Extract,    Flavoring,    What 

Constitutes  a  8 

Extract  of  Ginger   44 

Extract  of  Lemon   32-36 


Index 


81 


Extract  of  Mint  (Spear- 
mint)    49 

Extract  of  Orange   8,  41 

Extract  of  Peppermint 43 

Extract  of  Pistachio,  Imi- 
tation    59 

Extract  of  Rose  46 

Extract  of  Sarsaparilla   ...  49 

Extract  of  Vanilla 10-25 

Extract  of  Wintergreen  ...  43 
Extraction  of  Vanilla  Beans  17 
Extracts  by  Maceration  and 

Percolation  8 

Extracts      from      Essential 

Oils  8 

Extracts  from  Esters  8 

Extracts  from  Synthetics . .  8 
Extracts,  Non- Alcoholic. 27,  28 

Federal  Standard  for  Al- 
mond Extract  42 

Federal  Standard  for  Ex- 
tract of  Anise 47 

Federal  Standard  for  Cas- 
sia Extract  48 

Federal  Standard  for  Cel- 
ery Extract  47 

Federal  Standard  for  Clove 
Extract  49 

Federal  Standard  for  Cin- 
namon Extract  48 

Federal  Standard  for  Gin- 
ger Extract  44 

Federal  Standard  for  Lem- 
on Extract  32 

Federal  Standard  of  Oil  of 
Lemon 32 

Federal  Standard'  for  Pep- 
permint Extract  43 

Federal  Standard  for  Rose 
Extract  46 

Federal  Standard  for  Spear- 
mint Extract  49 

Federal  Standard  for  Tonka 
Extract  25 

Federal  Standard  for  Ter- 
peneless  Lemon  Extract.  34 

Federal  Standard  for  Va- 
nilla Extract 23 

Federal  Standard  for  Win- 
tergreen Extract  43 

Figuring  Costs  of  Extract 
Department 76,  77,  78,  79 


Filling  Bottles   74,  5 

Filter     and     Percolator, 

Double  Pressure  59,  60 

Filtering  Liquids  56,  57 

Filtering  Papers    55,  56 

Filters   55-60 

Filtration  54-60 

Filtration  Methods 54-60 

Finished  Extracts,  Care  of.  31 
Flavoring     Extract,     What 

It  Is  8 

Fluid  Measure 71 

Formula   for  Allspice    (Pi- 
mento)  Extract   47 

Formula  for  Celery  Ext. ...  48 
Formula  for  Chocolate  Ex- 
tract      49 

Formula  for  Clove  Ext 49 

Formula    for    Making   Va- 
nilla Extract  22,  23 

Formula     for     Peppermint 

Extract  44 

Formula   for   Almond    Ex- 
tract    42,  43 

Formula  for  Anise  Extract  47 
Formulas      for     Cinnamon 

Extract 48 

Formulas    for   Ginger   Ex- 
tract   ;..:.44,  45,  46 

Formula  for  Imitation  Sar- 
saparilla Extract 49,  50 

Formulas    for   Lemon   Fla- 
vor, Imitation 41 

Formulas  for  Imitation  Pis- 
tachio Extract  50 

Formulas     for     Rose     Ex- 
tract    46,  47 

Formulas    for    Terpeneless 

Lemon  Extract 38,  39 

Formulas   for  Wintergreen 

Extract  43 

Fruit  Acid  Solution 68 

Fruit  Oils  51 

Gas  in  Aqua-Ammonia 64 

Ginger  Extract 8,  44,  45,  46 

Graduating  Containers 69 

Grinding  Vanilla  Beans 17 

Guadeloupe  Vanilla  Beans.  II 

Harrop  on  Flavoring  Ext.  24 
Hot      Work      in      Extract 
Making    27 


82 


Index 


Household  Ammonia 72 

Howard  Method  for  Essen- 
tial Oils  64 

Imitation  Extracts  8,  9,  26 

Imitation  Lemon  Flavor...  40 

Imitation  Pistachio  Ext 50 

Imitation   Sarsaparilla  Ext.  49 
Imitation  Vanilla  Extract..  26 

Java  Vanilla  Beans 12 

Labeling  Imitation  Ext 28 

Laboratory  Notes    52-56 

Lemon  Extract 8,  32-36 

Lemon  Ext.,  Fed.  Standard  32 

Lemon  Extract,  Mfg 32-36 

Lemon  Flavor,  Imitation. . .  40 
Lemon     Flavor,     Imitation, 

Formulas   41 

Lemon  Oil 32,  33 

Maceration  in  Vanilla  Bean 
Exhaustion 19 

Machines  for  Cutting  Va- 
nilla Beans  17 

Machine  for  Mechanical 
Maceration  of  Vanilla 
Beans  20,  21 

Manufacture  of  Lemon  Ex- 
tract   32-36 

Manufacture  of  Terpene- 
less  Extract  of  Lemon. 34-39 

Manufacture  of  Vanilla  Ex- 
tract   10-25 

Manufacture  of  Various 
Extracts  42-49 

Mauritius  Vanilla  Beans...   n 

Meat  Cutters  for  Vanilla 
Beans  17 

Mechan.  Maceration  Proc- 
ess for  Vanilla  Beans ...  22 

Menstruums  for  Vanilla 
Bean  Exhaustion 18 

Methods  for  Testing  Oils, 

61,  62,  63 

Mexican  Vanilla  Beans n 

Mint  Extract  49 

Miscellaneous   Extracts..  .42-49 

Miscellaneous  Recipes 67-69 

Non-Alcoholic   Extracts. 27,  28 
Nutmeg  Extract 8 


Oil  of  Lemon 32,  33 

Oil     of     Lemon,     Federal 

Standard  of  32 

Oil  of   Orange 32 

Oil  Testing 61,  62,  63 

Orange  Extract  8,  41 

Orange  Oil  33 

Peach  Extract,  Imitation . .     9 

Peppermint  Extract  8,  43 

Percolating  Process  in  Va- 
nilla Bean  Exhaustion. 20,  22 
Percolation  in  Vanilla  Bean 

Exhaustion 18,  19 

Percolators  for  Testing  Va- 
nilla Beans  '. .  16 

Pimento  (Allspice)  Ext...  47 
Pineapple  Ext,  Imitation..  9 
Pistachio  Ext,  Imitation...  50 

Plain  or  Simple  Syrup 67 

Proof  Spirit 52 

Purchasing  Vanilla  Beans.  16 
Purifying  Essential  Oils...  66 

Qualifications  of  a  Manu- 
facturer    7 

Qualitative  Tests  for 
Water  54 

Raspberry  Ext.,  Imitation.  9 
Record  of  Costs,  Extract 

Department   77,  78 

Remington  on  Maceration.  19 
Remington  on  Percolation.  19 

Resins  14 

Rose  Extract i,  8,  46,  47 

Rule  for  Diluting  Alcohol.  53 

Sarsaparilla  Extract  49 

Sassafras  Ext,  Imitation..  9 
Sealing  Wax  Formulas.  .68,  69 

Selecting  Vanilla  Beans 15 

Seychelles  Vanilla  Beans. ..   li 

Soda  Foam,  Formula 67 

Solution,  Fruit  Acid 68 

Spearmint  Extract 49 

Standard,  Federal,   Extract 

of  Almond  42 

Standard,  Federal,  for  An- 
ise Extract  47 

Standard,  Federal,  for  Cas- 
sia Extract  48 

Standard,  Federal,  for  Cel- 
ery Extract  47 


Index 


Standard,  Federal,  for  Cin- 
namon Extract  48 

Standard,  Federal,  for  Clove 
Extract 49 

Standard,  Federal,  for  Gin- 
ger Extract  44 

Standard,  Federal,  for 
Lemon  Extract  32 

Standard,  Federal,  Oil  of 
Lemon  32 

Standard,  Federal,  for  Pep- 
permint Extract  43 

Standard,  Federal,  for  Rose 
Extract  46 

Standard,  Federal,  for 
Spearmint  Extract 49 

Standard,  Federal,  for  Ter- 
peneless  Lemon  Extract.  34 

Standard,  Federal,  for 
Tonka  Extract  25 

Standard,  Federal,  for  Va- 
nilla Extract 23 

Standard,  Federal,  for 
Wintergreen  Extract 43 

Storaging  of  Vanilla  Beans  16 

Strawberry  Extract,  Imita- 
tion of  9 

Synthetical  Extracts  8 

Syrup    Formula    67 

Syrup  Table 71 

Tables  of  Weights  and 
Measures  71 

Tahiti  Vanilla  Beans 12 

Terpeneless  Extract  of 
Lemon  8,  34-39 

Terpeneless  Lemon  Ext, 
Federal  Standard  34 

Terpeneless  Lemon  Ext., 
Formulas  38,  39 

Terpeneless  Orange  Ext...     8 

Test  Percolators  for  Va- 
nilla Beans  16 

Testing  Oil  of  Lemon    62 


Testing  Oil  of  Cloves 62 

Testing  Oil  of  Almond   ...  62 

Testing  Methods 61,  62,  63 

Testing  Otto  of  Roses 63 

Testing  Vanilla  Extract...  31 

Tests  for  Water,  Rules 54 

Thyme  Extract  8 

Tonka  Extract 8,  25 

Tonka      Extract,      Federal 
Standard   25 

U.  S.  Definition  of  Flavor- 
ing Extracts    8 

Use   of   Coloring 40 

Vanilla  Beans   10,  n,  15 

Vanilla  Bean  Exhaustion..  17 

Vanilla  Bean  Storage 16 

Vanilla  Beans,  Varieties 

10,  n,  12,  13 

Vanilla  Beans,  Where  Cul- 
tivated    10 

Vanilla  Extract 8,  10,  25 

Vanilla     Extract,     Federal 

Standard   23 

Vanilla   Ext,   Formula.. 22,  23 
Vanilla   Extract,   Manufac- 
ture    10-25 

Vanilla  Extract,  Testing...  31 

Vanilla  Resins 15 

Vanillin 8,  13,  14,  25,  26,  28 

Vanilla  Extract  8,  26 

Varieties  of  Vanilla  Beans  10 

Various  Extracts   42-49 

Vinegar    65 

Water  Tests 54 

Weights      and      Measures, 

Tables  71 

What  Constitutes  a  Flavor- 
ing Extract 8 

White  Vanilla  27 

Wintergreen  Extract 8,43 


84  Practical  Flavoring  Extract  Maker 


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Practical  Flavoring  Extract  Maker 


85 


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86  Practical  Flavoring  Extract  Maker 


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